Sciencemadness Discussion Board

Issues with Soxhlet set up

A.Fleming - 12-1-2018 at 12:11

I've never used Soxhlet apparatus before and I have troubles understanding how to properly perform the following step from my protocol:

To a gently refluxing suspension of 1 g Lithium aluminium hydride in 100 mL of diethyl ether, there was added 1.2 g of compound as a saturated diethyl ether solution with use of a Soxhlet extraction condenser which is modified allowing the continuous return of condensed solvent (through the thimble). After the addition was complete, the refluxing conditions were maintained."

Soo... How do I do it? I run RBF with condenser on top until reflux stabilizes and then I open it, add Soxhlet with compound and continue refluxing or I set up everything cold (RBF with LAH+ether + Soxlet with compound in ether + condenser) and then start refluxing?

Thanks

happyfooddance - 12-1-2018 at 13:43

I'm sure you would get more help if you specified what "compound" is... Because the answer depends on what "compound" is. This doesn't seem like a typical soxhlet extraction, and this seems like you are running a reaction with a soxhlet to help with the reaction, but unless you specify what "compound" is, you are not likely to any help, because nobody know's what "compound" could be if you don't say.

JJay - 12-1-2018 at 13:49

It sounds like they suspended 1 g of LiAlH4 in 100 mL of ether in a flask (250 mL probably) and then placed 1.2 g of the compound in a thimble and put it in a Soxhlet and then attached the Soxhlet to the top of the flask and a reflux condenser to the top of the Soxhlet then started refluxing. LiAlH4 and ether are dangerous substances to play around with, even in such small quantities, unless you know what you're doing.

[Edited on 13-1-2018 by JJay]

NEMO-Chemistry - 12-1-2018 at 14:03

Quote: Originally posted by JJay  
It sounds like they suspected 1 g of LiAlH4 in 100 mL of ether in a flask (250 mL probably) and then placed 1.2 g of the compound in a thimble and put it in a Soxhlet and then attached the Soxhlet to the top of the flask and a reflux condenser to the top of the Soxhlet then started refluxing. LiAlH4 and ether are dangerous substances to play around with, even in such small quantities, unless you know what you're doing.

Would this be used so the solvent was colder when it reached the compound?

I ask because i got two types, one has a very thing bottom, its supposed to help warm the solvent in the soxhlet while it fills up. The other has a thicker bottom and dosnt get the solvent in the soxhlet warm.

I dont know but from what you just said, it dosnt sound like something to mess with unless you know the ins and outs of it first.

Ether is a funny thing, i used it alot with no problems. I kind of treated it alot like DCM in the end, then one day about 100ml went up and to this day i have no idea what made it burn.

happyfooddance - 12-1-2018 at 14:16

Quote: Originally posted by JJay  
It sounds like they suspected 1 g of LiAlH4 in 100 mL of ether in a flask (250 mL probably) and then placed 1.2 g of the compound in a thimble and put it in a Soxhlet and then attached the Soxhlet to the top of the flask and a reflux condenser to the top of the Soxhlet then started refluxing. LiAlH4 and ether are dangerous substances to play around with, even in such small quantities, unless you know what you're doing.


But it doesn't say that, it says 1.2g of "compound" in a saturated ether sol... It sounds not like an extraction but a synthesis...

aga - 12-1-2018 at 14:17

Sounds like more of a Practical question.

Stick the stuff in the soxhlet part, surrounded by filter paper.
Bung the condenser on top, hook up the coolant pipes.

Add X amount of solvent to the flask that will be boiling the solvent - remember there has to be more than enough to fill the upper part.

Add some solvent to the upper part to avoid airlocks - basically enough to get some solvent into the syphon tube.

Turn on the juice and see what shakes loose.

NEMO-Chemistry - 12-1-2018 at 15:02

I dont understand the modified part, if you modify a soxhlet so it returns constantly, then its.......

Unless
The 1.2g is in the soxhlet as stated in a solution, the soxhlet dosnt empty fully (thats the mod), so the solvent drips into thimble and a small amount returns to the flask.

I guess you could get funky with glass and sort something, i dont know how you would mod a soxhelt to just drip back a little everytime some solvent drips into it.

Maybe try and rig something with a dean stark?

I smell fried onions ;)

[Edited on 12-1-2018 by NEMO-Chemistry]

A.Fleming - 12-1-2018 at 15:42

Quote: Originally posted by happyfooddance  
I'm sure you would get more help if you specified what "compound" is... Because the answer depends on what "compound" is. This doesn't seem like a typical soxhlet extraction, and this seems like you are running a reaction with a soxhlet to help with the reaction, but unless you specify what "compound" is, you are not likely to any help, because nobody know's what "compound" could be if you don't say.


My bad, of course.
I`m trying to convert β-unsaturated nitro compound into saturated amine.
β-nitro stryrene to be precise.

I`m completely unfamiliar with Pd/C approach, nor do i have the equipment.
Other sources suggest iron as possibility. Never researched such options. I have a nice Allihn condenser and Sohxlet to match.

The reflux is supposed to last for 48 hours - i guess the idea here is to slowly add the styrene to LAH with use os sohxlet. But i don`t get the modification of thimble - why use thimble at all? I understand the styrene must dissolve bad in ether, so why not fill sohxlet with saturated solution of styrene (no thimble) and let the refluxed ether dilute the styrene and add it dropwise to th RBF, where LAH awaits. Am I reading this wrong?

[Edited on 12-1-2018 by A.Fleming]

[Edited on 12-1-2018 by A.Fleming]

[Edited on 12-1-2018 by A.Fleming]

JJay - 12-1-2018 at 16:38

You ought to watch a YouTube video showing how a Soxhlet extractor works.

Vosoryx - 12-1-2018 at 18:01

You might get a more friendly and helpful response if you were to dispel lingering concerns of cookery.

Going from beta-nitro styrene to the corresponding fully saturated amine would be VERY close to amphetamine. Perhaps you already knew this, as this is what you are trying to make? Or maybe you aren't trying to make this. LiAlH4 is hard to get, and not necessary for this reduction - a good cook would know this. On the other hand, you have a post history of two, and signed up the same day.

The point is that we don't know. Convince us, and some of the more knowledgeable members might be able to offer some assistance.

Edit:

I was wrong - it wouldn't be very close to an amphetamine. It would be an amphetamine. (Took me a minute to visualize that.) If I recall correctly, this method (Substituted nitrostyrene reduced using LiAlH4)is identical to the one provided in Alexander Shulgin's: "PIHKAL".
Correct me?

[Edited on 13-1-2018 by Vosoryx]

NEMO-Chemistry - 12-1-2018 at 18:45

Did I mention i smelled onions frying?

Actually i got to be honest and say i think i get this now.

I think i was spot on. As mentioned if you watch a soxhlet it fills up completely then empties entirely. The compound is dissolved in ether and put into a thimble in the soxhlet. So you got a soxhlet with a thimble of liquid in.... Whats going to happen as soon as it fills?

Its going to dump the lot in one go into the pot. If you were doing certain naughty things, you wouldnt want this if doing it this way would you? NO.

So as i said the modification is to block part of the return in the soxhlet, this way it just drips non stop. So your solvent reaches the condenser and drops on the compound, the exact same amount from the thimble is then returned to the pot.

This is why its 48 hours, you reflux really slow. the rate should match the soxhlet volume. I am going to guess and say this was done with a 250ml soxhlet, if i got the sums right then it would take roughly 42 hours for the thimble to have had delivered 250ml of solvent at a very slow rate.

So the reaction actually takes place in the soxhlet, if that makes sense. If it dosnt then go search certain books on interesting compounds that are closer than precursors to stuff that might get you in trouble.

EDIT LOL the post above was posted as i was doing mine! SNAP

Yeah i saw the same book reference, hence the reference to it being closer than a precursor!

BUT funny how i am crap at chemistry but that kind of chemistry is easy to understand!

[Edited on 13-1-2018 by NEMO-Chemistry]

NEMO-Chemistry - 12-1-2018 at 18:50

So yes use your condesor on top of a soxhlet, dont bother with the mod and a thimble, keep a fire blanket handy though.

BTW do more reading, there is a trip up with the phenethylamines

sorry but when i google this look what pops up
http://onlinelibrary.wiley.com/doi/10.1002/0471264180.os023....
[Edited on 13-1-2018 by NEMO-Chemistry]

[Edited on 13-1-2018 by NEMO-Chemistry]

A.Fleming - 13-1-2018 at 03:53

I know how it looks like - random guy pops here with 0 post and asks very fishy questions :D I`ve been moderator and administrator to different forums (not chem related, but still) and i know the idea.
I`ll come up with better response probably in the evening as i`m in the hurry right know, but to sum up :
- i have 10 years of lab experience (including PhD) but it was a molecular biology lab, not pure organic chemistry. I have some experience, but organic chem is a field i want to improve right know.
- i have no problems with getting equipment and chemicals as i run my own chem-related company so i can order anything i want as long as it fits with my company profile
- i do understand the idea behind Soxhlet extraction but this is a different use of it, so i decided i`d ask you guys. I THINK that the idea here is to have a very slow addition of the reagent to the hydride, but the modification puzzles me.
- if you REALLY need to know, i`m trying to explore my very own pet project that resolves around alternative pathways of diaminopyrimidine chemotherapeutics, hence the aromatic aldehydes
- i KNOW what can be made out of substituted aromatic compounds, trust me, i had to fill out the forms while ordering it. I`ve no interest in amphetamine synthesis or any other illicit use of those compounds.

This is a technical challenge for me. I sequenced genome of some god forsaken plant but nobody ever told me how to properly recrystallize stuff, i learned it all for my self.

Last edit - it took me a while to get the "onions frying" metaphor :)

[Edited on 13-1-2018 by A.Fleming]

[Edited on 13-1-2018 by A.Fleming]

[Edited on 13-1-2018 by A.Fleming]

NEMO-Chemistry - 13-1-2018 at 04:28

Quote: Originally posted by A.Fleming  
I know how it looks like - random guy pops here with 0 post and asks very fishy questions :D I`ve been moderator and administrator to different forums (not chem related, but still) and i know the idea.
I`ll come up with better response probably in the evening as i`m in the hurry right know, but to sum up :
- i have 10 years of lab experience (including PhD) but it was a molecular biology lab, not pure organic chemistry. I have some experience, but organic chem is a field i want to improve right know.
- i have no problems with getting equipment and chemicals as i run my own chem-related company so i can order anything i want as long as it fits with my company profile
- i do understand the idea behind Soxhlet extraction but this is a different use of it, so i decided i`d ask you guys. I THINK that the idea here is to have a very slow addition of the reagent to the hydride, but the modification puzzles me.
- if you REALLY need to know, i`m trying to explore my very own pet project that resolves around alternative pathways of diaminopyrimidine chemotherapeutics, hence the aromatic aldehydes
- i KNOW what can be made out of substituted aromatic compounds, trust me, i had to fill out the forms while ordering it. I`ve no interest in amphetamine synthesis or any other illicit use of those compounds.

This is a technical challenge for me. I sequenced genome of some god forsaken plant but nobody ever told me how to properly recrystallize stuff, i learned it all for my self.

Last edit - it took me a while to get the "onions frying" metaphor :)

[Edited on 13-1-2018 by A.Fleming]

[Edited on 13-1-2018 by A.Fleming]

[Edited on 13-1-2018 by A.Fleming]


The soxhlet adaptation is as I mentioned, ironically the best information is on the cook sites! Personally I think I would try a different approach. But if you want to try the soxhlet then the idea is to lift the bottom hole up.

I can think of a couple of ways to do this, most would ruin the soxhlet. So I think the bigger clue is in the thimble part, most thimbles are of two types, one type is porous and the other has a hole in the bottom.

If you watch a soxhlet, you see it empties the entire thing each time, this is because the outlet is at the bottom. So the adaptation has to be something that raises the outlet so the soxhlet only empties a little each time.

I looked at my Thimbles and I think you got two realistic choices that are easy to do. Use a thimble that is non porous and block the bottom hole of it, then put a small hole near to the top level of the Soxhlet point where it triggers the siphon.

This way the thimble fills up and leaks into the main body of the soxhlet, eventually it will reach the siphon point and empty the Soxhlet.

However most the contents of the thimble will not empty as it can only empty down to the thimble hole.

The other way need a smaller thimble, same idea but you put a tube from the bottom hole in the thimble, terminate this tube just below siphon point.

Its slightly harder to do, but it means you will be taking solution from the bottom of thimble each time and not the top. I think this will also speed things up. No idea if I can bodge a pic to explain, but I will try.

My skills at computer art really suck!

Might be a good idea to fully explain next time, as this method is mentioned in the litrature almost exclusively for meth making.
I will be back with a rough pic
EDIT

I just figured an easier way, using two thimbles BRB

Can you see what I mean now? The inner thimble is porous at bottom so solvent goes through all product. Comes out of bottom and into the outer thimble, the outer thimble is shorter than inner, but higher than siphon point.

So eventually outer thimble spills into soxhlet, after a while the spill over will reach siphon and empty the soxhlet, but it will only empty the contents of soxhlet which is all spill over.

This is why it takes so long, inner thimble only leaks from bottom so all product in contact with solvent.

sox5.png - 147kB

[Edited on 13-1-2018 by NEMO-Chemistry]

[Edited on 13-1-2018 by NEMO-Chemistry]

sox6.png - 149kB

unionised - 13-1-2018 at 05:33

Quote: Originally posted by JJay  
You ought to watch a YouTube video showing how a Soxhlet extractor works.

Why?
The OP explicitly says that the Soxhlet has been modified so it doesn't work the way it would in a TY video.

LearnedAmateur - 13-1-2018 at 06:30

Quote: Originally posted by Vosoryx  
You might get a more friendly and helpful response if you were to dispel lingering concerns of cookery.

Going from beta-nitro styrene to the corresponding fully saturated amine would be VERY close to amphetamine. Perhaps you already knew this, as this is what you are trying to make? Or maybe you aren't trying to make this. LiAlH4 is hard to get, and not necessary for this reduction - a good cook would know this. On the other hand, you have a post history of two, and signed up the same day.

The point is that we don't know. Convince us, and some of the more knowledgeable members might be able to offer some assistance.

Edit:

I was wrong - it wouldn't be very close to an amphetamine. It would be an amphetamine. (Took me a minute to visualize that.) If I recall correctly, this method (Substituted nitrostyrene reduced using LiAlH4)is identical to the one provided in Alexander Shulgin's: "PIHKAL".
Correct me?

[Edited on 13-1-2018 by Vosoryx]


If it’s just beta nitrostyrene then the corresponding amine would be phenylethylamine, amphetamine would require another methyl group (for simplicity sake, isopropyl as opposed to 1,2-ethyl). Completely legal to possess, I usually buy a couple of hundred grams at a time for personal use over a few months. However, the amounts produced here wouldn’t even be enough for a single dose, so I don’t see the concern unless it’s a substituted nitrostyrene.. Not enough to warrant cookery claims IMO, considering the knowledge of chemistry shown.

[Edited on 13-1-2018 by LearnedAmateur]

JJay - 13-1-2018 at 07:06

Quote: Originally posted by unionised  
Quote: Originally posted by JJay  
You ought to watch a YouTube video showing how a Soxhlet extractor works.

Why?
The OP explicitly says that the Soxhlet has been modified so it doesn't work the way it would in a TY video.


The type of extraction a Soxhlet does is referred to as "continuous solvent extraction." Where exactly are you seeing that the Soxhlet wouldn't work the way it would in a YT video?

More to the point, the OP said he had never used a Soxhlet before and was having trouble understanding how one works.

A.Fleming - 13-1-2018 at 12:49

Quote: Originally posted by NEMO-Chemistry  

Can you see what I mean now?
[Edited on 13-1-2018 by NEMO-Chemistry]

[Edited on 13-1-2018 by NEMO-Chemistry]


YES! Thank you so much for your hard work here. I need to think on this with clear head but for now your idea involves the least glass molding and the addition of compound should be slow enough. I just need some decent thimbles now, nice :)
Quote: Originally posted by Vosoryx  
Not enough to warrant cookery claims IMO, considering the knowledge of chemistry shown.
[Edited on 13-1-2018 by LearnedAmateur]

Thank you.
Quote: Originally posted by JJay  
Quote: Originally posted by unionised  
Quote: Originally posted by JJay  
You ought to watch a YouTube video showing how a Soxhlet extractor works.

Why?
The OP explicitly says that the Soxhlet has been modified so it doesn't work the way it would in a TY video.

The type of extraction a Soxhlet does is referred to as "continuous solvent extraction." Where exactly are you seeing that the Soxhlet wouldn't work the way it would in a YT video?
More to the point, the OP said he had never used a Soxhlet before and was having trouble understanding how one works.


I have no trouble understanding the soxhlet extraction, quite the opposite - i admire the idea, its simplicity and efficiency. What i couldn`t understand was how to modify said soxhlet so it goes more into continuous and less "batchy" system of work. More drop-wise, less "down-goes-the-full-volume-of-soxhlet-into-RBF" mode ;) Also - this is a synthesis use of soxhlet, not the usual extraction.
Now i have some idea to work with, thanks to NEMO.


[Edited on 13-1-2018 by A.Fleming]

JJay - 13-1-2018 at 13:55

What exactly makes you think that this isn't the full-volume-of-soxhlet-into-rbf style? I know it says "modified" Soxhlet, but it doesn't say "simple reflux extractor" (which I guess would be called a Payen extractor and predates the Soxhlet).

Vosoryx - 13-1-2018 at 17:42

Quote: Originally posted by LearnedAmateur  

If it’s just beta nitrostyrene then the corresponding amine would be phenylethylamine, amphetamine would require another methyl group...


Alas, I was wrong. You're right - whoops.

I apologize for this.

unionised - 14-1-2018 at 13:51

Quote: Originally posted by JJay  
What exactly makes you think that this isn't the full-volume-of-soxhlet-into-rbf style? I know it says "modified" Soxhlet, but it doesn't say "simple reflux extractor" (which I guess would be called a Payen extractor and predates the Soxhlet).


What makes me think that is the quote in the OP which says it isn't.
i.e. " a Soxhlet extraction condenser which is modified allowing the continuous return of condensed solvent (through the thimble).".
A Soxhlet doesn't do continuous extraction it's intermittent.
What the synthesis needs is a continuous, slow, addition of the material. A Soxhlet which adds none for ages and then a whole lot at once is the equivalent of trying to titrate using a tomato ketchup bottle.
It may well mean something more like Payen's idea.

JJay - 14-1-2018 at 14:26

Quote: Originally posted by unionised  
A Soxhlet doesn't do continuous extraction it's intermittent.


Whatever, dude. The only part that isn't continuous is the addition of the solvent to the flask below. I'm getting tired of your incessant and pointless questions, unionized.

http://oleoresins.melbia.com/principle-of-soxhlet-extraction...

"Soxhlet extraction is a continuous solid/liquid extraction."

JJay - 14-1-2018 at 14:47

Taking "modified" Soxhlet and "continuous" return of solvent too literally isn't necessarily the writer's intent.

See https://books.google.com/books?id=Vz39BAAAQBAJ&pg=PA523#... for example, which describes a similar use of a Soxhlet. Do you really think the author intended that a distillation flask containing LiAlH4 be placed below the Soxhlet?


SWIM - 14-1-2018 at 15:34

The actual answer, guys.

This is a question only somebody who was in O-chem a few decades ago is likely to know the answer to.

Soxhlet extractors are not designed the way they were when Schulgin posted that recipe.

There was no external siphon tube. The siphon tube was an integral part of the thimble. This means you could just break the siphon tube off the thimble and the liquid would continuously drip through the thimble.

The extractor body was just open inside top to bottom, and the thimble was hung in there on a wire through holes at the top of the thimble.

This means even if you've got old-time extraction thimbles (I do) you can't use them as Schulgin did without the old style Soxhlet body.

I'm not saying there aren't some clever ways around this as suggested above, but the Schulgin ref is about breaking the integral siphon off the old-style thimble. Seriously, check out the original paper and I believe he makes it explicit. If not, he did elsewhere in his writings.

EDIT: Somebody posted here recently that they have a 1980s Aldrich, or Sigma, or some such catalogue.
That catalogue may be old enough to have old style Soxhlets listed in it.

[Edited on 14-1-2018 by SWIM]

JJay - 14-1-2018 at 15:48

Quote: Originally posted by SWIM  
The actual answer, guys.

This is a question only somebody who was in O-chem a few decades ago is likely to know the answer to.

Soxhlet extractors are not designed the way they were when Schulgin posted that recipe.

There was no external siphon tube. The siphon tube was an integral part of the thimble. This means you could just break the siphon tube off the thimble and the liquid would continuously drip through the thimble.

The extractor body was just open inside top to bottom, and the thimble was hung in there on a wire through holes at the top of the thimble.

This means even if you've got old-time extraction thimbles (I do) you can't use them as Schulgin did without the old style Soxhlet body.

I'm not saying there aren't some clever ways around this as suggested above, but the Schulgin ref is about breaking the integral siphon off the old-style thimble. Seriously, check out the original paper and I believe he makes it explicit. If not, he did elsewhere in his writings.

EDIT: Somebody posted here recently that they have a 1980s Aldrich, or Sigma, or some such catalogue.
That catalogue may be old enough to have old style Soxhlets listed in it.

[Edited on 14-1-2018 by SWIM]


According to the information that is available on this topic, that does not seem to be the case. This paper has a copy of Soxhlet's original drawing of his extractor, which was considered a "modification" of Payen's extractor. What is the Shulgin reference here?

Nm... this is clearly Shulgin's mescaline synthesis... why the heck would you use a Soxhlet for that?

Attachment: ed084p1913.pdf (85kB)
This file has been downloaded 454 times

[Edited on 15-1-2018 by JJay]

SWIM - 14-1-2018 at 21:04

I'm not saying anything about Soxhlet's original invention.

I'm just talking about a kind of Soxhlet design which was common back then ( !980s and before) but has since been so totally superseded by extractors with external siphons that they've plain disappeared. I really don't know when this form was developed either, so I don't know how long they were around.

I didn't recall what phenylethylamine he used to it make, but I thought it was something more exotic than mescaline.
I recall it was used to introduce the nitrostyrene into the LAH. (Schulgin was always trying to up his yield from LAH reductions. He tried all sorts of inert atmospheres, even helium. I believe he started to favor THF over ether for its greater solvent power.)

I also thought I recalled that the nitrostyrene in that reaction was somewhat gooey and insoluble, thus mandating the gradual extraction. But I read that long ago and it wasn't a matter of great interest to me so I really don't remember it all that well.

Anyway his description involved breaking the siphon off the thimble in the paper I read. I am pretty confident of that. Could there be more than one published account where he describes this?

I'll check. I'm sure it's in PIHKAL because that's the only Schulgin I've bothered to read.


But seriously, these suckers were the sole pattern sold by at least one US company (Aldrich?), and I don't recall seeing any ones back then similar to what everybody makes now.

NEMO-Chemistry - 15-1-2018 at 04:26

I dont know enough chem to get involved in the arguing. I do know the synth isnt Mescaline, the synth that shugin used this apparatus for was a solid dissolved in a liquid, it needed a solvent slowly added and warmed.

What SWIM describes is exactly what the thing i drew does. I based it on an old extractor i have seen, the extractor was used by someone i know (genuinely not me) to replicate some the recipes. The person in question should be easy to find online, they taught chemistry and they are now on holiday at HER MAJ's pleasure.

SWIM - 15-1-2018 at 13:39

Quote: Originally posted by NEMO-Chemistry  
I dont know enough chem to get involved in the arguing. I do know the synth isnt Mescaline, the synth that shugin used this apparatus for was a solid dissolved in a liquid, it needed a solvent slowly added and warmed.

What SWIM describes is exactly what the thing i drew does. I based it on an old extractor i have seen, the extractor was used by someone i know (genuinely not me) to replicate some the recipes. The person in question should be easy to find online, they taught chemistry and they are now on holiday at HER MAJ's pleasure.



Thanks for convincing me I'm not insane, NEMO-Chemistry. I looked far and wide on the internet for a picture of one of those. but no luck.

I was starting to think I had brought that thing with me from some parallel dimension and forgot about it.

As for the chem details, I was just trying to explain what I thought I recalled off the reference. It is not unlikely that I'm wrong on the details.
Tried looking through Schulgin last night, found 2 places where he does the soxhlet thing, but neither was the one with the explanation I thought I remembered.

I recall now that I have read a few of his papers in Jacs, or Nature or something like that, and those might differ from the reports in PIHKAL.

JJay - 15-1-2018 at 16:04

Quote: Originally posted by NEMO-Chemistry  
I dont know enough chem to get involved in the arguing. I do know the synth isnt Mescaline, the synth that shugin used this apparatus for was a solid dissolved in a liquid, it needed a solvent slowly added and warmed.



I'm not trying to get involved in any arguing either, but if you take a look look at Shulgin's mescaline synth, you should be able to make a rational decision on whether or not this is that synth.

I think Eleusis is usually accurate but is often to be taken with a grain of salt (and Zwitterion is Eleusis' sock puppet, right?), but this is what he had to say about using a Soxhlet with LiAlH4 reductions: https://erowid.org/archive/rhodium/chemistry/eleusis/zwit.2c...

He made a saturated solution of the nitrostyrene and added it in small portions to an almost-full Soxhlet, or at least he claimed he did.

S.C. Wack - 15-1-2018 at 19:53

Nitrostyrenes of all kinds were reduced from the beginning of LAH by leaching out of Soxhlets; it's standard technique when solubility is this low. A little blockage in the drain tube just right can gum up the purge. EDIT: or pressure-equalized addition funnel.

[Edited on 16-1-2018 by S.C. Wack]

PirateDocBrown - 15-1-2018 at 22:03

Quote: Originally posted by SWIM  
The actual answer, guys.

EDIT: Somebody posted here recently that they have a 1980s Aldrich, or Sigma, or some such catalogue.
That catalogue may be old enough to have old style Soxhlets listed in it.

[Edited on 14-1-2018 by SWIM]


Sadly, my 1988 Aldrich shows a Wheaton Soxhlet in the modern style.
But I have seen the old style extractors myself, long ago. Never used one.

SWIM - 15-1-2018 at 22:17

Been thinking about the conversion thing.

If you just drill or grind a hole in the bottom of the body of a modern Soxhlet, it will continuously drip through the hole and work like the Schulgin-mentioned modification did.

If the hole can be plugged up with an appropriate sized plug of something inert like teflon or glass it'll again function like a regular Soxhlet.

So a hole that takes a reasonably tight PTFE stopper would let the extractor do either job. The seal on the hole wouldn't need to be perfect, just good enough so leakage into the boiling flask was a small fraction of the total flow.

NEMO-Chemistry - 16-1-2018 at 04:29

Quote: Originally posted by JJay  
Quote: Originally posted by NEMO-Chemistry  
I dont know enough chem to get involved in the arguing. I do know the synth isnt Mescaline, the synth that shugin used this apparatus for was a solid dissolved in a liquid, it needed a solvent slowly added and warmed.



I'm not trying to get involved in any arguing either, but if you take a look look at Shulgin's mescaline synth, you should be able to make a rational decision on whether or not this is that synth.

I think Eleusis is usually accurate but is often to be taken with a grain of salt (and Zwitterion is Eleusis' sock puppet, right?), but this is what he had to say about using a Soxhlet with LiAlH4 reductions: https://erowid.org/archive/rhodium/chemistry/eleusis/zwit.2c...

He made a saturated solution of the nitrostyrene and added it in small portions to an almost-full Soxhlet, or at least he claimed he did.


The red herring is Phikal here, yes the mescaline thing mention what your talking about. I did double check, but the modification he did and used in this case wasnt in PHIKAL, i think it must have been a paper.

To explain how I know its not mescaline......

The person in question was a chem teacher, i knew them through a relation of theirs, at no point did i meet them in a teaching capacity.

But on a visit to the relation, i was taken to meet them and see the lab, being interested in chemistry who isnt going to go tour someones lab???

Like me the guy liked Cacti, except he specifically liked the stone type where i like them all. We spoke about the fact that in the UK everyone in power seems utterly oblivious to the fact, most garden centres sell the peyote cactus!!

Whats more most people in the UK have never heard of Mescaline, its not a major drug here. The guy however liked messing with the chemistry and Mescaline, so i know he extracted it directly from the cactus.

He would have no need to do the synth in Phikal in the way its done. What he showed me i didnt understand fully, it isnt meth but i would guess its a derivative. I do know its pretty dangerous, and from what I was told it isnt something you would take more than a couple of times.

The comment about arguing was aimed at the fact, i am so under qualified to even begin to say people are right or wrong, but this occasion I am 100% positive the soxhlet adaptation refers to what I drew.

Its just one those things that fix in your mind for no apparent reason, maybe it just impressed me how much time and effort, this clever teacher devoted to messing his head up.

He was a really nice guy, reminds me alot like some of you with his knowledge. Very likeable and willing to talk for hours about chemistry, as a side note he isnt that old (maybe mid-late 40's) but having seen my grandad with parkinsons, this guy has it for sure.

oh one last nugget
The Soxhlet thing came about because like me, he loved collecting odd old chem glass. I got loads of it I havnt a clue what it does!!

JJay - 16-1-2018 at 05:00

Quote: Originally posted by NEMO-Chemistry  
Quote: Originally posted by JJay  
Quote: Originally posted by NEMO-Chemistry  
I dont know enough chem to get involved in the arguing. I do know the synth isnt Mescaline, the synth that shugin used this apparatus for was a solid dissolved in a liquid, it needed a solvent slowly added and warmed.



I'm not trying to get involved in any arguing either, but if you take a look look at Shulgin's mescaline synth, you should be able to make a rational decision on whether or not this is that synth.

I think Eleusis is usually accurate but is often to be taken with a grain of salt (and Zwitterion is Eleusis' sock puppet, right?), but this is what he had to say about using a Soxhlet with LiAlH4 reductions: https://erowid.org/archive/rhodium/chemistry/eleusis/zwit.2c...

He made a saturated solution of the nitrostyrene and added it in small portions to an almost-full Soxhlet, or at least he claimed he did.


The red herring is Phikal here, yes the mescaline thing mention what your talking about. I did double check, but the modification he did and used in this case wasnt in PHIKAL, i think it must have been a paper.

To explain how I know its not mescaline......

The person in question was a chem teacher, i knew them through a relation of theirs, at no point did i meet them in a teaching capacity.

But on a visit to the relation, i was taken to meet them and see the lab, being interested in chemistry who isnt going to go tour someones lab???

Like me the guy liked Cacti, except he specifically liked the stone type where i like them all. We spoke about the fact that in the UK everyone in power seems utterly oblivious to the fact, most garden centres sell the peyote cactus!!

Whats more most people in the UK have never heard of Mescaline, its not a major drug here. The guy however liked messing with the chemistry and Mescaline, so i know he extracted it directly from the cactus.

He would have no need to do the synth in Phikal in the way its done. What he showed me i didnt understand fully, it isnt meth but i would guess its a derivative. I do know its pretty dangerous, and from what I was told it isnt something you would take more than a couple of times.

The comment about arguing was aimed at the fact, i am so under qualified to even begin to say people are right or wrong, but this occasion I am 100% positive the soxhlet adaptation refers to what I drew.

Its just one those things that fix in your mind for no apparent reason, maybe it just impressed me how much time and effort, this clever teacher devoted to messing his head up.

He was a really nice guy, reminds me alot like some of you with his knowledge. Very likeable and willing to talk for hours about chemistry, as a side note he isnt that old (maybe mid-late 40's) but having seen my grandad with parkinsons, this guy has it for sure.

oh one last nugget
The Soxhlet thing came about because like me, he loved collecting odd old chem glass. I got loads of it I havnt a clue what it does!!



I have absolutely no idea what you're talking about. The wording of the OP's post appears to be lifted verbatim Shulgin's mescaline synthesis scaled at 50% with the name of the nitrostyrene removed. There are various reasons why I don't think the "modification" is the one you drew, but I'm not trying to beat a dead horse on this topic.

NEMO-Chemistry - 16-1-2018 at 06:02

Quote: Originally posted by JJay  
Quote: Originally posted by NEMO-Chemistry  
Quote: Originally posted by JJay  
Quote: Originally posted by NEMO-Chemistry  
I dont know enough chem to get involved in the arguing. I do know the synth isnt Mescaline, the synth that shugin used this apparatus for was a solid dissolved in a liquid, it needed a solvent slowly added and warmed.



I'm not trying to get involved in any arguing either, but if you take a look look at Shulgin's mescaline synth, you should be able to make a rational decision on whether or not this is that synth.

I think Eleusis is usually accurate but is often to be taken with a grain of salt (and Zwitterion is Eleusis' sock puppet, right?), but this is what he had to say about using a Soxhlet with LiAlH4 reductions: https://erowid.org/archive/rhodium/chemistry/eleusis/zwit.2c...

He made a saturated solution of the nitrostyrene and added it in small portions to an almost-full Soxhlet, or at least he claimed he did.


The red herring is Phikal here, yes the mescaline thing mention what your talking about. I did double check, but the modification he did and used in this case wasnt in PHIKAL, i think it must have been a paper.

To explain how I know its not mescaline......

The person in question was a chem teacher, i knew them through a relation of theirs, at no point did i meet them in a teaching capacity.

But on a visit to the relation, i was taken to meet them and see the lab, being interested in chemistry who isnt going to go tour someones lab???

Like me the guy liked Cacti, except he specifically liked the stone type where i like them all. We spoke about the fact that in the UK everyone in power seems utterly oblivious to the fact, most garden centres sell the peyote cactus!!

Whats more most people in the UK have never heard of Mescaline, its not a major drug here. The guy however liked messing with the chemistry and Mescaline, so i know he extracted it directly from the cactus.

He would have no need to do the synth in Phikal in the way its done. What he showed me i didnt understand fully, it isnt meth but i would guess its a derivative. I do know its pretty dangerous, and from what I was told it isnt something you would take more than a couple of times.

The comment about arguing was aimed at the fact, i am so under qualified to even begin to say people are right or wrong, but this occasion I am 100% positive the soxhlet adaptation refers to what I drew.

Its just one those things that fix in your mind for no apparent reason, maybe it just impressed me how much time and effort, this clever teacher devoted to messing his head up.

He was a really nice guy, reminds me alot like some of you with his knowledge. Very likeable and willing to talk for hours about chemistry, as a side note he isnt that old (maybe mid-late 40's) but having seen my grandad with parkinsons, this guy has it for sure.

oh one last nugget
The Soxhlet thing came about because like me, he loved collecting odd old chem glass. I got loads of it I havnt a clue what it does!!



I have absolutely no idea what you're talking about. The wording of the OP's post appears to be lifted verbatim Shulgin's mescaline synthesis scaled at 50% with the name of the nitrostyrene removed. There are various reasons why I don't think the "modification" is the one you drew, but I'm not trying to beat a dead horse on this topic.


Actually you do have a point.

I have a bias in this, in the UK Mescaline from this route would be insane, the cactus is so common and cheap why on earth would anyone go the route the OP wants?

But thats the UK, AFAIK few if anyone is bothered about Mescaline, i have never heard of it as a street drug here.

The cactus is cheap and common in garden centers. But other countries the opposite is true, unless the OP comes clean we wont ever know.

But i do agree its a perfect fit for Mescaline, its just to me this would be really stupid. Plus I am assuming the OP is being semi clever and heading down the more interesting substance route.

It isnt flogging a dead horse by a long way, i have enjoyed the reading and double checking, i have also learnt alot from it.

Ok its drug related, but chemistry is chemistry to me. Plus it isnt often i can contribute in a meaningful way :D.

Makes me wonder if i should a export business for cactus lol! JOKING

LearnedAmateur - 16-1-2018 at 11:28

Quote: Originally posted by NEMO-Chemistry  
[
He would have no need to do the synth in Phikal in the way its done. What he showed me i didnt understand fully, it isnt meth but i would guess its a derivative. I do know its pretty dangerous, and from what I was told it isnt something you would take more than a couple of times.


I just want to add that mescaline can’t really be considered a derivative of methamphetamine, under the implication that ‘derive’ means to get from A to B, only that it is structurally related as a substituted phenylethylamine. Firstly, methamphetamine has a geminal methyl group on the alpha carbon, there would be no way to remove this reliably in order to get to n-methylphenylethylamine. Secondly, it would be incredibly difficult to tack on the three methoxy groups, or to introduce three hydroxyl groups to react with a methylating agent (which would also react with the amine without sufficient protection); as R groups are ortho, para directing, I can’t see how you’d be able to add a substituent to the meta position (since mescaline is 2,3,4 methoxyphenylethylamine) without heavy modification to the base molecule which is far above my level of knowledge. As far as I know, it’s pretty much impossible to get from an amphetamine to a phenylethylamine without destroying the entire molecule and starting from benzene or toluene - most ‘easy’ syntheses of mescaline, what would be used for street production, would likely start with plant sources such as gallic acid or vanillin for example, where some or all of the aromatic substituents are already in place.

unionised - 16-1-2018 at 11:53

Quote: Originally posted by JJay  


Whatever, dude. The only part that isn't continuous is the addition of the solvent to the flask below. I'm getting tired of your incessant and pointless questions, unionized.



The only part of this use of a Soxhlet that actually does what the synthesist wants is "the addition of the solvent to the flask below".

It's hardly "pointless" to explain that the bit of kit you use to do something has to be set up to do it properly.

(Incidentally, it wasn't a question, pointless or otherwise).

A.Fleming - 16-1-2018 at 13:17

You guys really write faster than i have the time to process all this.
Had i known your view on mescaline i would approach this whole topic differently.
Schulgins` mescaline synthesis is a solid inspiration here, yes, but definitely not a goal, I`ll explain later.
Quote: Originally posted by SWIM  
Been thinking about the conversion thing.
If you just drill or grind a hole in the bottom of the body of a modern Soxhlet, it will continuously drip through the hole and work like the Schulgin-mentioned modification did.
If the hole can be plugged up with an appropriate sized plug of something inert like teflon or glass it'll again function like a regular Soxhlet.
So a hole that takes a reasonably tight PTFE stopper would let the extractor do either job. The seal on the hole wouldn't need to be perfect, just good enough so leakage into the boiling flask was a small fraction of the total flow.


Interesting! With succesful drill i`d have my original soxhlet and a modified one if needed. I`m thinking of fusing your idea with NEMOs`.
Quote: Originally posted by JJay  
Quote: Originally posted by NEMO-Chemistry  


I have absolutely no idea what you're talking about. The wording of the OP's post appears to be lifted verbatim Shulgin's mescaline synthesis scaled at 50% with the name of the nitrostyrene removed. There are various reasons why I don't think the "modification" is the one you drew, but I'm not trying to beat a dead horse on this topic.


But thats the UK, AFAIK few if anyone is bothered about Mescaline, i have never heard of it as a street drug here.
But i do agree its a perfect fit for Mescaline, its just to me this would be really stupid. Plus I am assuming the OP is being semi clever and heading down the more interesting substance route.
It isnt flogging a dead horse by a long way, i have enjoyed the reading and double checking, i have also learnt alot from it.
Ok its drug related, but chemistry is chemistry to me. Plus it isnt often i can contribute in a meaningful way :D.

I honestly laughed at "semi clever" xD Yes, i`m trying to head down to more interesting routes (i hope) but mescaline is not one of them. And i hid the name of styrene, since it would be extremely straightforward for you. It`s 3,4,5-trimethoxystyrene.
I`m looking into trimethoprim direction - i hope the structure alone can defend me. If i seem shady it`s mainly due to my lack of confidence in organic chemistry, i know the chemicals i use are very close to some VERY interesting yet illicit substances and i do believe i have an research idea that is worth investing time and effort in. I don`t want to talk much about the idea alone as it is not that well researched (yet) by me but mainly i don`t know you guys and i have no idea which of you might have biotech education or business connections. Am i paranoid?

I basically got what i wanted here, but i don`t want to be THAT guy and disappear after the topic is over... I think i`ll stay, there is so much i can learn here - this forum is NEAT!

DJF90 - 16-1-2018 at 13:31

Quote: Originally posted by A.Fleming  
Yes, i`m trying to head down to more interesting routes (i hope) but mescaline is not one of them. And i hid the name of styrene, since it would be extremely straightforward for you. It`s 3,4,5-trimethoxystyrene.


You know that reduction of 3,4,5-trimethoxy-beta-nitrostyrene will give you mescaline, right?

JJay - 16-1-2018 at 14:00

Quote: Originally posted by A.Fleming  
You guys really write faster than i have the time to process all this.
Had i known your view on mescaline i would approach this whole topic differently.
Schulgins` mescaline synthesis is a solid inspiration here, yes, but definitely not a goal, I`ll explain later.

Quote: Originally posted by SWIM  
Been thinking about the conversion thing.
If you just drill or grind a hole in the bottom of the body of a modern Soxhlet, it will continuously drip through the hole and work like the Schulgin-mentioned modification did.
If the hole can be plugged up with an appropriate sized plug of something inert like teflon or glass it'll again function like a regular Soxhlet.
So a hole that takes a reasonably tight PTFE stopper would let the extractor do either job. The seal on the hole wouldn't need to be perfect, just good enough so leakage into the boiling flask was a small fraction of the total flow.


Interesting! With succesful drill i`d have my original soxhlet and a modified one if needed. I`m thinking of fusing your idea with NEMOs`.
Quote: Originally posted by JJay  
Quote: Originally posted by NEMO-Chemistry  


I have absolutely no idea what you're talking about. The wording of the OP's post appears to be lifted verbatim Shulgin's mescaline synthesis scaled at 50% with the name of the nitrostyrene removed. There are various reasons why I don't think the "modification" is the one you drew, but I'm not trying to beat a dead horse on this topic.


But thats the UK, AFAIK few if anyone is bothered about Mescaline, i have never heard of it as a street drug here.
But i do agree its a perfect fit for Mescaline, its just to me this would be really stupid. Plus I am assuming the OP is being semi clever and heading down the more interesting substance route.
It isnt flogging a dead horse by a long way, i have enjoyed the reading and double checking, i have also learnt alot from it.
Ok its drug related, but chemistry is chemistry to me. Plus it isnt often i can contribute in a meaningful way :D.

I honestly laughed at "semi clever" xD Yes, i`m trying to head down to more interesting routes (i hope) but mescaline is not one of them. And i hid the name of styrene, since it would be extremely straightforward for you. It`s 3,4,5-trimethoxystyrene.
I`m looking into trimethoprim direction - i hope the structure alone can defend me. If i seem shady it`s mainly due to my lack of confidence in organic chemistry, i know the chemicals i use are very close to some VERY interesting yet illicit substances and i do believe i have an research idea that is worth investing time and effort in. I don`t want to talk much about the idea alone as it is not that well researched (yet) by me but mainly i don`t know you guys and i have no idea which of you might have biotech education or business connections. Am i paranoid?

I basically got what i wanted here, but i don`t want to be THAT guy and disappear after the topic is over... I think i`ll stay, there is so much i can learn here - this forum is NEAT!



You should probably learn how to quote posts properly, especially if you want people to believe that you have a PhD and aren't synthesizing mescaline.

zed - 16-1-2018 at 16:06

Peyote cacti have been in high demand, for generations in the US.

Once upon a time, they grew large, wild, and free... in Mexico and the American South-West.

A decade or two ago, some folks reported to me, that this was no longer the case. Confronted with high demand, and slow growth cycle, the wild cacti had become quite rare.
And, the physical size of found samples, had devolved to...tiny.

So, freely available in commerce, in the UK? Surprised!

NEMO-Chemistry - 16-1-2018 at 16:50

Quote: Originally posted by zed  
Peyote cacti have been in high demand, for generations in the US.

Once upon a time, they grew large, wild, and free... in Mexico and the American South-West.

A decade or two ago, some folks reported to me, that this was no longer the case. Confronted with high demand, and slow growth cycle, the wild cacti had become quite rare.
And, the physical size of found samples, had devolved to...tiny.

So, freely available in commerce, in the UK? Surprised!
Now I got to go and double check!!!
I started collecting cacti before i can really remember, I was given my grandads collection after he died, apparently i would spend hours looking at them.

They have always fascinated me, but i havnt purchased any for around 4 years.

But certainly 4 years ago ANY garden center or even DIY super stores that sold plants, sold them. Mainly just labeled as stone cactus, but I would guess 70%+ of them were peyote, mostly in the 1.5-2 inch range.

Whats really funny, i used by loads of them, if you cut the main body off the root stock its a great grafting base for harder cactus! Whats annoying with them though, if you graft with them the bugger grow back on the side of the stump!

I am told a few long ago hippies in the UK used Mescaline, it was also used in psychiatric hospitals up until the 70's i think.
But apart from that......Zero interest in UK as far as I can tell.

LSD was the favored drug, according to my ex hippy mum. Who swears she never touched it, but her eyes twitch ;). From the descriptions i would of thought Mescaline would have been preferred, Also called the god drug??

I am also informed one the reasons it wasnt liked was awful nausea when taking it, but to me this would be down to piss poor isolation.

My interest inst drugs, but plants are a big interest, funny to think we got to reflux and mess about for hours, when a little cactus does it without fuss and a brain with no problem! Gotta love plants..

Yeah I am too trusting and assumed the OP was on the level, i wished i could remember the name of the other drug now. Now making that would of been clever!

Why dosnt anyone try and synth stuff like Kuri Kuri or however you spell it. I think vets use a derivative to this day as a anesthetic.
Or natural herbicides, jesus whats wrong with life people want to get out of it so badly??

SWIM - 16-1-2018 at 16:58

Quote: Originally posted by zed  
Peyote cacti have been in high demand, for generations in the US.

Once upon a time, they grew large, wild, and free... in Mexico and the American South-West.

A decade or two ago, some folks reported to me, that this was no longer the case. Confronted with high demand, and slow growth cycle, the wild cacti had become quite rare.
And, the physical size of found samples, had devolved to...tiny.

So, freely available in commerce, in the UK? Surprised!


I can understand your surprise, but I think 'the cactus' he was referring to was San Pedro or one of the other fast growing mescaline bearing cacti.
(Peruvianus, etc)

They can grow from a few inches to 6 feet in a few years, as opposed to the 50 or 75 years or something it takes peyotes to get to a decent size.
They get huge given enough time, and they grow in all kinds of weather and climate. Alkaloid levels can be much lower, but the poundage makes up for it to those who grow it for such purposes.

I've also heard and read of the scarcity of peyote today. Supposedly it's almost impossible to find large ones in the US now. Seems a lot of harvesters in the 60s and later didn't know to just cut the top off and leave the root to grow another, or even a cluster.

EDIT: I see NEMO wasn't talking about San Pedro or other columnar mescaline bearing cacti. My mistake.


[Edited on 17-1-2018 by SWIM]

JJay - 16-1-2018 at 18:08

I suspect that water-retaining substances in cacti make it hard to obtain dry samples for solvent extractions or to prepare aqueous extracts. It's not quite as simple as "Buy cacti. Chop up cacti in blender. Filter cactus juices. Basify. Extract with diethyl ether. Evaporate water to obtain freebase alkaloids." It's more like "Buy cacti. Dry sliced cacti in dessicator for two months. Mangle cactus pieces in mortar and pestle. Place cactus pieces in blender. Grind cacti to fine powder. Replace burned-out blender. Extract with dilute hydrochloric acid. Filter gelatinous mass through glass sinter under vacuum for several hours to obtain a few mL of gooey filtrate. Throw clogged glass sinter at the wall in frustration."

I have not personally tried this, but I am pretty sure that only professional research laboratories actually extract mescaline from cacti.

NEMO-Chemistry - 16-1-2018 at 19:08

Here they use those fruit dryer things for shrooms, they were legal to own and cultivate until a couple of years ago.
The law said you could pick them, keep them but not eat them!! Then after 50 years maybe more, they decided that perhaps just banning them would be best.......

Which reminds me, October I found my first ever false Morel in our wood! I really wanted to pick it and extract it, but dont fancy messing with it TBH. We do have a yellow mushroom that gives a strong dye like turmeric in colour, a really nice yellow.

Cant find it in my books, so no idea how dangerous it is. It dosnt smell that good though.

Oh and the San Pedro is pretty difficult to get here, you have to buy from a specialist nursery, and at least for me, they dont grow very well here.

[Edited on 17-1-2018 by NEMO-Chemistry]

LearnedAmateur - 17-1-2018 at 07:02

Does the smell remind you of hospital disinfectant? I know that certain species like the Angel’s Bonnet produce iodoform which is a strong yellow similar to turmeric, and you are able to detect its presence by the smell of the mushroom alone.

NEMO-Chemistry - 17-1-2018 at 11:22

Quote: Originally posted by LearnedAmateur  
Does the smell remind you of hospital disinfectant? I know that certain species like the Angel’s Bonnet produce iodoform which is a strong yellow similar to turmeric, and you are able to detect its presence by the smell of the mushroom alone.


Hospitals this century smell of IPA. But I have smelt Iodoform, in a way it does kind of smell like that but with a more nasty undertone. The colour is stunning however.

LearnedAmateur - 17-1-2018 at 13:41

Yeah I guess things have changed, it’s just that I’ve just heard of it being referred to as such, I don’t really think there’s anything else to compare it to, not in my experience anyway. Seems understandable, most mushrooms, fungi in general for that matter, that I’ve come across don’t exactly have pleasant odours. Just thought that may help you to narrow it down a bit.

NEMO-Chemistry - 18-1-2018 at 13:44

Quote: Originally posted by LearnedAmateur  
Yeah I guess things have changed, it’s just that I’ve just heard of it being referred to as such, I don’t really think there’s anything else to compare it to, not in my experience anyway. Seems understandable, most mushrooms, fungi in general for that matter, that I’ve come across don’t exactly have pleasant odours. Just thought that may help you to narrow it down a bit.

Nah just messing with you, I know the smell you mean, and yes it is a bit like that.

Though smell is so different between people, i love NO2, the smell to me is just like a strong swimming pool. No one else at home can stand the slightest hint of it.

Alot of the mushrooms around here smell really 'woody', or a kind of deep earth smell. We seem to have an overabundance of deadly ones though.

A.Fleming - 19-1-2018 at 15:11

Wow, i love the direction of the off-topic you guys went :D
But getting a little back on the topic - i visited some of my old friends in organic chemistry institute, they recommended me some top shelf lab glass blower (90 year old veteran) but he was absent, so after over 5 hours of searching for the right guy i left the building with a headache and one thing in mind.
Syringe pump.
My inspiration was shulgin`s protocol, yes, but things have moved on since then and instead of modifying the old school soxlet, i think i`ll try 2-neck RBF. One neck with condenser, i`ll use Allihn after shulgin, although i was suggested to to use graham as it is more efficient for ether. January is tight in terms of money, so allihn will it be, i`ll use lots of dry ice and test on just ether to see if it`s enough. second neck will lead to syringe pump which will add saturated solution of compound in drops, over hours. Very steady addition. I need to calculate volumes right, i think i`ll add all of compound in 36 hours, then reflux it for another 12.
My only concern is that the solubility of compound (i have to check it yet) in cold ether (as i can`t imagine hot ether syringes!) will be very low and it will take a lot of syringes to add it completely.
The biggest one i should be able to borrow from my friends is 60 ml, i need to do some tests and math now :)
What do you guys think?

[Edited on 19-1-2018 by A.Fleming]

[Edited on 19-1-2018 by A.Fleming]

[Edited on 19-1-2018 by A.Fleming]

[Edited on 19-1-2018 by A.Fleming]

JJay - 19-1-2018 at 16:15

I think you're making mescaline.

NEMO-Chemistry - 19-1-2018 at 21:42

I think your better buying it, cheaper, much quicker. Your way isnt going to work well, i dont think your Mescaline like that though, i think your aiming for black tar crap. But JJay could be right, it could be Mescaline, but me thinks i got him this time! I am 99.9% sure your target with that method is black crap.

Oh and a nice warm house......If your skint how come you can afford a very large amount of ether your going to use?

[Edited on 20-1-2018 by NEMO-Chemistry]

S.C. Wack - 20-1-2018 at 09:37

I think he's making people react. If he actually had the nitrostyrene, ether, and LAH, the target is fire.

SWIM - 20-1-2018 at 10:25

He's gonna use dry ice and a Graham condenser for ether???
Don't think this poster is exactly lab-savvy.
Don't think he's ever used either ether. (Used ether either, sorry.)

But isn't the point of this modification so you can use less ether to dissolve reactants for the reaction?

If just adding a saturated solution really slowly is all you're after, then break out one of those constant addition funnels.
Those suckers are just worlds apart from regular pressure compensating addition funnels for this kind of thing.

S.C. Wack - 20-1-2018 at 11:37

Check the original literature of Ramirez and Burger, and Nystrom and Brown, which is on Rhodium and elsewhere. The pressure equalizing funnel I mentioned earlier is for the side arm which is much like the Soxhlet's.

NEMO-Chemistry - 24-1-2018 at 19:15

Ether is nothing to worry about, until you open the bottle

zed - 26-1-2018 at 15:01

When working with LiAlH4, it is important to be a control freak.

Therein I am not wild about using a Soxhlet in the process. There is the potential for a loss of homeostasis. Since your ether is already refluxing.... How will your LiAlH4, respond to the automatic addition of more reactant? Perhaps, not well.

That being said, I had friends who utilized the Soxhlet/LiAlH4/DiethylEther technique, perhaps 40-50 times, without serious incident. Number 51, was their unlucky number.

A small building disappeared.

It went like this. A Graham condenser cools pretty well, but isn't very good for a reflux like this. Quite possibly, it becomes backed-up with distillate, and it floods.

So, the Soxhlet was outfitted with an Allihin. Which is a decent condenser, but not very good for ether, because it allows too much to escape.

A long uncooled extension tube is affixed to the top of the Allhin, in an attempt to improve ether retention. The tube extends outside, and above roof level. It did not work well enough.

During the hydrolysis stage of the reduction, things got hot, and ether loss reached a critical juncture. There was either no reserve ether, or no way to safely get it into the hot slurry.

Hot ether vapor and hydrogen, vented through the extension tube, fast. Pressure built up. The tube is emitting a loud didgirydoo type sound. This interesting harmonic effect attracts the interest of neighbors, and concerns them enough, that they call the local authorities for reassurance.

My compatriots, courageous young chemists, but no fools.... Exit the building. At just about that time, Public Safety Workers arrive, internal pressure forces the apparatus apart, the building quickly fills with ether vapor and hydrogen gas..... And Kabloouie!

This made the local papers, and arrests were made. Now, the laws were different in those days. And eventually, with the assistance of lots of lawyer money, the fair-haired boys avoided prosecution.

Awful lot of trouble ensued, over a shortage of ether, and lack of an adequate condenser.

If you are gonna run this reaction, either use a high-tech condenser, or have a 24/40 female, welded to the top of your Soxhlet's Allihin. This will allow you to attach an auxillary condensor, and thereby retain yer pretty face.

NEMO-Chemistry - 26-1-2018 at 15:11

If you want to get some safer practice in first, distill a gallon of petrol on a camp stove. If you manage that OK then have a go with the synth.