Sciencemadness Discussion Board - Distillation Setup for 1,4-Butanediol to gamma-Butyrolactone

Distillation Setup for 1,4-Butanediol to gamma-Butyrolactone

Chemrock - 3-1-2010 at 09:52

Any recommendations on the easiest distillation apparatus setup for distilling GBL from a filtered BDO+CuCrO4 slurry ?
I have cooked the BDO and the CuCrO4 for 3 hours at 200 deg C, and have filtered the majority of the CuCrO4 out via a coffee filter. Now I need to distill to obtain the GBL.

[Edited on 3-1-2010 by Chemrock]

[Edited on 3-1-2010 by Chemrock]

User - 3-1-2010 at 10:02

Cooking.......................?
Forget it man.

Cooks are like rats , they dont die easily.

[Edited on 3-1-2010 by User]

Chemrock - 3-1-2010 at 10:20

Sorry I should have said refluxed instead of cook, my bad

DJF90 - 3-1-2010 at 10:30

Take your pots and pans elsewhere; we aren't interested in helping your kind!

entropy51 - 3-1-2010 at 10:59

Quote: Originally posted by Chemrock

Sorry I should have said refluxed instead of cook, my bad

If you don't how to set up a distillation setup and you're trying to make GBL, you're probably a cook no matter how you say it.

Chemrock - 3-1-2010 at 11:15

There are a lot of ways to set up a distillation. My question was as to the simplest for the process I described based on anyones experience. For example is it necessary to perform fractional distillation in the process. What type of condenser would be sufficient, ie West, Graham,Liebig etc. Is it necessary to water cool or can air cool suffice.

For example would the setup shown on this link be sufficient:

http://www.unitedglasstech.com/Monthly_Specials.htm

Thanks for any advice

turd - 3-1-2010 at 11:36

I don't know that particular synthesis, but I guess ideally you would use a small column (10-20 cm). A glass blower will make you a Hempel column for ~$20. Apart from that the apparatus you posted looks nice. Also I'm not sure how stable gamma-hydroxybutyrolactone (GBL) is. In case it is unstable at higher temperatures you might want to use a vacuum source, an aspirator should do. Of course you need a good heat source and preferably a magnetic stirrer.

Edit: An important aspect is the scale you're operating on. If you're working on the 10g scale, you need special "micro" distillation apparatuses. For 100g batches the posted apparatus should be fine, but additional 100ml and 250ml round bottom flask would be a nice thing to have.

PS: I wonder if an industrial solvent like GBL is worth the trouble - but it sounds like a nice first chemistry project.

PPS: The witch-hunt here is getting to ridiculous levels. From the FAQ:

Quote:

Mad Science is about [...] Things Man was Not Meant to Know. More prosaically, Mad Science is about exploring and manipulating aspects of the natural world without the facilities or resources of "sane science" as practiced in academic, industrial, and governmental research settings.
[...]
Mad Scientists are drawn like moths before a candle to the most dangerous areas of exploration: energetic, corrosive, and bioactive materials.

Sounds like Chemrock is more in the spirit of the site than the academic wanks...

[Edited on 3-1-2010 by turd]

User - 3-1-2010 at 11:58

Also to help someone clueless that just after a direct precursor to GHB...
Right..

entropy51 - 3-1-2010 at 12:26

From the FAQ:

Quote:

It is okay to be ignorant when first arriving and posting. However, you must be willing to make an effort to learn. Additionally, certain topics are unwelcome no matter what section they are posted in. The discussion of criminal activities or weapons production is inappropriate. Heed this warning or face merciless taunting.

GBL is a List 1 Chemical.

Chemrock - 3-1-2010 at 12:44

I've noticed

turd - 3-1-2010 at 13:00

*shrug*
Where I live its legal to possess (and make) unlimited amounts of GBL as long as it's stored correctly. So your "List 1" might not be as important as you think.

Back on topic: The plastic clamps suck, I've managed to melt those during distillation.

Get ones made from metal.

entropy51 - 3-1-2010 at 14:40

Quote: Originally posted by turd

Where I live its legal to possess (and make) unlimited amounts of GBL as long as it's stored correctly. So your "List 1" might not be as important as you think.

Sez you. Chemrock says he's in San Francisco, and it's not legal there. The taunting will continue.

Polverone, could we get a better class of cooks around there? GHB is such crap.

Chemrock - 3-1-2010 at 14:45

Based on the number of views this topic has generated I would say that my interest is shared by many. After all it is a "discussion board" not an interview forum for the next Pope

entropy51 - 3-1-2010 at 14:51

Quote: Originally posted by Chemrock

Based on the number of views this topic has generated I would say that my interest is shared by many. After all it is a "discussion board" not an interview forum for the next Pope

WTF, you're not just a newbie, you're dense too. Views? Try looking at the posts. Not exactly a heartwarming response, huh?

Views? Most drivers slow down to gawk at auto accidents. I suppose you believe all of them think highway fatalities are a good thing and aspire to become one.

[Edited on 3-1-2010 by entropy51]

Chemrock - 3-1-2010 at 14:56

The world is full of pleasant people unfortunately you're not one of them.

entropy51 - 3-1-2010 at 15:17

Quote: Originally posted by Chemrock

The world is full of pleasant people unfortunately you're not one of them.

Good grief! If you think me not pleasant, you wouldn't enjoy the comaraderie of a prison at all, so maybe you should refrain from naughty chemistry, lest you get yourself locked up in a very unpleasant place.

[Edited on 4-1-2010 by entropy51]

Sedit - 3-1-2010 at 15:52

LOL sorry buddy but I must laugh.... He really said "Cooked the BDO" LMAO, sorry but that is to funny.

DJF90 - 4-1-2010 at 13:37

Hahahaha good one entropy... I actually had a U2U exchange with this guy after he was complaining about my post to him... well it looks like he took some notice of what I said and has cleaned up a little... but seriously... GBL? I can think of nicer, and more legitimate ways of getting into amateur chemistry.

Chemrock: If you're serious about getting into chemistry as an amateur hobby, then stick around. Just chose some more sane projects and you'll be a lot better off, people will be more interested in your work and you'll get alot from it. A good set of glass with ground joints is pretty essential if you're into serious organic synthesis, and will prove valueable over time if not instantly.

JohnWW - 4-1-2010 at 13:56

I suppose Chemrock's philosophy is: "If something is illegal, it must be good for you". There is some truth in this, however, because in many places drugs, including ones with analgesic or naturopathic or other pharmacological value, including non-alkaloidal ones like 1,4-butanediol and GBL and GBH and pot, have been made illegal by an abuse of legi$lative process, in the form of massive lobbying and bribery (often disguised as "election campaign contributions") of Congre$$people (particularly in the U$A) and Parliamentarians by the big alcohol and tobacco and pharmaceutical companies, who see such rival drugs as threats to their "patches", i.e. to their own grossly-overpriced wares.

BTW, there is not really much point in converting 1,4-butanediol to GBL, to use as a recreational drug, because 1,4-butanediol (which is made industrially in large quantities for use as an industrial solvent, which should be in Ullmann) itself can be drunk for the same drug effect, comparable to ethanol.

[Edited on 5-1-10 by JohnWW]

psychokinetic - 4-1-2010 at 14:03

Quote: Originally posted by JohnWW

"If something is illegal, it must be good for you".

I could really go a good, relaxing, refreshing murderous spree right now.

turd - 4-1-2010 at 15:04

Quote: Originally posted by DJF90

GBL? I can think of nicer, and more legitimate ways of getting into amateur chemistry.

Actually that's close to the perfect project for an absolute beginner in organic chemistry:
* Harmless reagents
* Cheap reagents
* Refluxing
* Catalysis
* Distillation
* Not too small of a scale

In any case, definitely better than my career starter: chloroform and chloral-hydrate.

Sedit - 4-1-2010 at 17:40

[rquote=168880&tid=13208&author=turd
Actually that's close to the perfect project for an absolute beginner in organic chemistry:
* Harmless reagents
* Cheap reagents
* Refluxing
* Catalysis
* Distillation
* Not too small of a scale

In any case, definitely better than my career starter: chloroform and chloral-hydrate.[/rquote]

See turd the issue is people inhearited belief in what harmless means. There is also the issue of someones ability to make a consumable product without proper understanding and facilitys. But hey who the hell am I to judge im just putting the facts of the matter out there.

len1 - 4-1-2010 at 18:43

The sad truth is, if you made anything, be it drug related, be it bomb related, just anything, having it reality related would already make it above par on this forum

Sedit - 4-1-2010 at 21:41

Put that way len it sort of depresses me. I like to feel this is a forum of people who may have had experiance with the sometimes dangerous stuff I play with. If something goes wrong I would like to have somewhere to turn other then what I can look up on google myself.

If people are reading and not practicing there is no excuss IMO because money is no huge factor and with a little ingenuity alot of equipment can be made from things in the shed. Small projects can be performed and down the line these can be combined into bigger projects given puritys and abilitys.

:Sigh: stop depressing people Len

len1 - 4-1-2010 at 22:20

Quote:

If people are reading and not practicing there is no excuss IMO because money is no huge factor and with a little ingenuity alot of equipment can be made from things in the shed. Small projects can be performed and down the line these can be combined into bigger projects given puritys and abilitys.

I agree with you entirely. Unfortunately the only people who want to get off their butt and do the unglamorous work are those with a vested interest. i.e. drug cooks and bomb makers. This is the reason for an observation of Polverone's earlier that SM can never reach the level of the Hive. What united them there is a common purpose.

Depressing - yes, I find it depressing. But I cant find solace in an imaginary reality. Maybe others can, maybe its to their benefit, maybe its not so bad, so I will stop intruding.

[Edited on 5-1-2010 by len1]

entropy51 - 5-1-2010 at 06:51

Quote: Originally posted by len1

The sad truth is, if you made anything, be it drug related, be it bomb related, just anything, having it reality related would already make it above par on this forum

I thought the purpose of this forum was to get free references. That seems to be where the activity is.

Chemrock - 6-1-2010 at 10:37

Very interesting response by the board.
All I can add is that "curious minds have a need to know"
With over 400 anonymous views I would say that this topic was of a great interest to a lot of curious minds.
Thanks to all who contributed.

entropy51 - 6-1-2010 at 15:08

Quote: Originally posted by Chemrock

With over 400 anonymous views I would say that this topic was of a great interest to a lot of curious minds.

You deserve an attaboy! Give yourself a big pat on the back.

Vogelzang - 7-1-2010 at 16:15

The way I feel, I think if someone develops a drug problem or becomes an addict, it may have been his/her karma. If you prevented them from following their spiritual path then he/she might have to come back to live this type of lifestyle in their next life. People with drug and alcohol problems usually have to mature out of it before they can stay sober. I've known a lot of people like this, who had substance abuse problems, but later quit and avoided it completely for then on. We're all addicted to oil (petroleum) and most people are in denial about it.

Sedit - 7-1-2010 at 17:03

In a forum full of people with scientific minds you will have a better chance convincing them that drugs are not that bad then you will convincing them they will be reborn in a next life due to there Karmic influences.

Vogelzang - 7-1-2010 at 17:15

I know a number of people with science degrees that have religious and/or spiritual beliefs.

Sedit - 7-1-2010 at 19:42

Dont make it right thought.

len1 - 8-1-2010 at 04:51

Quote: Originally posted by entropy51

Quote: Originally posted by len1

The sad truth is, if you made anything, be it drug related, be it bomb related, just anything, having it reality related would already make it above par on this forum

I thought the purpose of this forum was to get free references. That seems to be where the activity is.

Which immediately leads to the question why is there so much activity in asking and posting references, when there is so little actually being done. My answer is that for many people this is a form of socializing. That explains many of the observation ive made before and the reactions to them.

[Edited on 8-1-2010 by len1]

sonogashira - 8-1-2010 at 05:22

Len, I don't see what is your concern. Over the years I have spoken with others in u2u, email etc. of the details of certain experiments... done some bad (due to lack of equipment) experiments of my own, given and received chemicals from other people for my/their experiments... but never once put any details of things I have done... because - quite honestly - it was nothing new, or clever, or worthwhile to share... just repeating experiments that have been written and presented in much nicer form in the journal references (which are still reports of people doing chemistry, after all!).
The pleasure I (and I'm sure others) get just from crystallizing copper sulfate, or bismuth (Many times, and many shapes!

)... or making simple esters which smell nice, or plastics in unimpressive powder form, is not necessarily interesting to others - yet still it is done, and not mentioned.

I can't imagine that people who have been here for years - who buy chemicals from whatever source - and ask for references on obscure reactions do it solely to socialize(!) - it is a very quite forum; and if that is the fact then they are in the wrong place!

For me it is sometimes enough to read of other (amateur or professional!) peoples interesting chemistry, and I think there is nothing wrong with that. Not everyone has the equipment or money to do impressive things... but dreaming costs nothing!

I wish it did not bother you so much Len... if the forum is a place to ask and to give help then that is enough I feel. Often I find that some of the help given here is better than what I could get at my university, so why not ask for help because it is all in the spirit of helping others towards the scientific endeavor, if it is reported here or to help someone who will later write a published paper - it is no matter!

turd - 8-1-2010 at 10:51

Quote: Originally posted by len1

Which immediately leads to the question why is there so much activity in asking and posting references, when there is so little actually being done.

One reason imay be that motivated newbies get immediately chased away by the local Taleban which disapproves of the subject or the lingo (c.f. this thread). What you end up with is a bunch of inbreeds patting themselves on the back for having superior goals. Which is of course just another type of being "kewl".

len1 - 8-1-2010 at 12:36

Crystalising copper sulphate, maybe. But havent seen references posted on that. With something just a bit more complicated it will soon be pretty obvious if youre doing it, because few things work straight away, esp as you say with bad equipment, and people ask for help describing what they did. There are plenty of examples of that in the past, see eg hydrazine thread. But that sort of thing's dried up now

Of course if they are cooking they are less likely to post .. but even then lots of 'swim' remarks abound.

Not to take it to hard? Should I get that noose of my neck then and climb down from the chair?

Sandmeyer - 8-1-2010 at 12:54

Quote: Originally posted by turd

Well said, well said...

sonogashira - 8-1-2010 at 13:59

Quote: Originally posted by len1

Not to take it to hard? Should I get that noose of my neck then and climb down from the chair?

Yes, step down Sir!

There are many more things to worry about... like people drinking industrial solvents! It is Friday night and this solvent-drinking is becoming an epidemic from what I can tell

Edit: And crystallizing bismuth is much more fun! I feel inspired to post some of my results now, but have this as a teaser

http://www.amazingrust.com/Experiments/how_to/Bismuth_Crysta...

and... http://www.bismuthcrystal.com/week.html

[Edited on 8-1-2010 by sonogashira]

[Edited on 9-1-2010 by sonogashira]

entropy51 - 8-1-2010 at 17:16

Quote: Originally posted by turd

One reason imay be that motivated newbies get immediately chased away by the local Taleban (sic) which disapproves of the subject or the lingo (c.f. this thread).

As always, Mr Turd has it arse backwards. The Taliban love drugs. That's the major source of their income! According to the NY Times the Taliban earned $ 300 million from the opium trade last year alone. Mr Turd should educate himself about where the money spent on illegal drugs goes. Then he wouldn't appear so dumb when he compares people who are against illegal drugs to the Taleban (sic).

crazyboy - 8-1-2010 at 18:16

Entropy, I respect you as a chemist and in the past you have contributed useful information to this forum but as of late your posts have turned decidedly judgmental and unproductive. Recently you haven't made a single post relating to chemistry, rather you attack anyone and everyone you even suspect of thinking about considering ordering a precursor to a watched chemical. I also disapprove of discussion by individuals who are clearly only interested in synthesizing drugs for profit or other sinister but that doesn't mean I berate them at every opportunity.

You are a bully, and quite frankly an asshole who seems to get pleasure from one or two sentence rebuttals insulting new members. In the future why don't you just keep your thoughts to yourself?

turd - 9-1-2010 at 01:38

Quote:

Mr Turd should educate himself

It fear it is you who is in dire need of some education.
1) On the ambiguous romanization and transcription of arabic
2) On reasoning by analogy. Apparently your intrusive thoughts concerning "illegal drugs" hamper your capability of abstraction.
3) Logical thinking. If it bothers you that drug money is going to the mafia, then you should support domestic made psychoactives. Every self-made g of speed is one g less for the mafia. Furthermore so far I didn't see you arguing pro-legalization. If I wasn't certain that you have OCD, I would believe that you are invested in "the business".

4) On the art of civilized discussion. Calling people "dumb" etc... does not make you "win" the argument. And a real discussion is not about being right anyway, but about sharing ideas.

My last post in this subthread. My best wishes to you, may you beat your demons one day. Good night.

Follow up on equipment

Chemrock - 18-1-2010 at 10:02

If anyone decides to order a distillation kit from United Glass Tech make sure to order a set of metal joint clamps ( not cheap at $45 for set of 5 ) because the green plastic ones that come in the kit are only temperature rated up to 140 Deg C. To attain proper distillation temps one will need to attain vapor temps in the column in excess of 200 Deg C. The metal clamps are rated up to 350 Deg C.

Also I don't recommend buying their clear 3/8 ID tubing because at $2.50/ft thats more expensive than 20 feet for $12.50 from Home Depot.

Bravo Sir!

mofookin - 22-9-2018 at 06:32

Quote: Originally posted by crazyboy

Entropy, I respect you as a chemist and in the past you have contributed useful information to this forum but as of late your posts have turned decidedly judgmental and unproductive. Recently you haven't made a single post relating to chemistry, rather you attack anyone and everyone you even suspect of thinking about considering ordering a precursor to a watched chemical. I also disapprove of discussion by individuals who are clearly only interested in synthesizing drugs for profit or other sinister but that doesn't mean I berate them at every opportunity.

You are a bully, and quite frankly an asshole who seems to get pleasure from one or two sentence rebuttals insulting new members. In the future why don't you just keep your thoughts to yourself?

I registered solely to agree with you, sir. This person of whom you speak does, in fact, appear to be a bully and an asshole, who attacks merely to attack. If the statement held no truth he wouldn't have made more than one or two posts here on a thread he adamantly disapproves of.

My hats off to you Crazyboy, for telling it how it is.

Funkerman23 - 22-9-2018 at 22:20

Quote: Originally posted by mofookin

Quote: Originally posted by crazyboy

You resurrected an 8 year old forum thread to agree with a long gone cook and then bash one of the more respected, and now sadly dead, member(s) here with your first post? Really, what the hell are you thinking. There is a glaring reason we kick cooks off of the forum: If they get arrested, they will try and blame this very forum for their crimes. We are on the margins more than any other academic group I can think of. Never mind how badly maligned and marginalized amateur chemistry still is. Never mind how many lives have been lost to illicit drug trade. Never mind the fact that this forum is the last refuge of the lone chemist either. Get a hint, Entropy was here long enough to see the same type of stupid behavior over and over again:What the hell do you expect? Him to support the very plague on our community?

mofookin - 27-9-2018 at 01:36

omg I am sorry I didn't know the history or date of the last post. my apologies. Alas, he did appear to pick on the man. Much like you are picking on me. for whatever reason. I do respect the dead though and am sorry I made the post now. has nothing to do with your ire, that I could give a shit about.

PS I'm neither a cook nor amateur chemist, I just like to read interesting stuff.

[Edited on 27-9-2018 by mofookin]