Sciencemadness Discussion Board

PPA extraction from proin chewable tablets

chemist1243 - 13-10-2020 at 07:26

I need to preface this with a warning;
This is NOT a discussion about the synthesis of drugs, and if anyone wants to talk about making amphetamines or other illicit substances, LEAVE. This about extracting a substance which has very little biological activity, and i dont consider it a drug in the same way amphetamine or cathinone is. I dont have a problem with drug synthesis discussion, but this is not the forum. Try TheVespairy or Hyperlab, they’ll like you more there.


I found an ingredient table for Proin, and dog medication in the form of chewable tablets which contain 25-75mg of PPA per tablets. I found a solubility table for PPA and the ingridents in proin chewables. Take a look:

https://core.ac.uk/download/pdf/145054785.pdf

https://dailymed.nlm.nih.gov/dailymed/getFile.cfm?setid=ea1b...

I made a solubility table, and I know that:

Soluble in alcohol:

PPA HCl dissolves in alcohol
Soy protein dissolves in alcohol

Insoluble in alcohol:

Stearic acid is insoluble
Silicon dioxide is insoluble

What i dont know is whatever the hell else everything is soluble in, like the protein, but i think i can get them out.


I did a methanol extraction 3x on the crushed up proin to get out the PPA and whatever else. It still had particles so i filtered them out to get a cloudy solution, which i filtered again to get a clear yellow solution. At this point i should have dissolved some fats and oils in the garlic and chicken liver, and some other crap, but I’d also have PPA. I can smell the garlic coming off the solution. I’m evaporating the methanol off to get what i believe will be an impure oily residue.

Now all i have to deal with is the fats and oils and the proteins like whey and soy protein. I’m going dissolve as much of the solution as i can in warm water, and then ill wash with stater fluid(crude, i know) to “defat” the solution. From there ill add sodium hydroxide to freebase the PPA HCl.

I’m gonna extract the aqueous solution with starter fluid to get out most of the PPA from the NaOH water. In the organic layer I’m expecting to have some proteins left, so ill wash the solution with salt water to pull anything polar out of solution, but also becuase apparently some proteins dissolve in salt solution much better than regular water. Ill dry the ether with anhydrous magnesium sulfate and extract out the PPA wit dilute HCl solution, which salts the freebase and pulls it into the aqueous layer. From there ill evaporate to either get
1: nothing
2: sticky/oily/gummy mess
3: crude PPA? Maybe :)

ill be reporting back with my findings soon.

Again, dont tell me what to do with the final product or turn this into a drug synthesis thread. Save it for the wasps if you catch my drift.

Later :D






arkoma - 13-10-2020 at 13:04

The Wasps know how to de-gakk pills, and "thou dost protest too much." Be advised that PPA is a List 1, if it matters.

I would be rather surprised if a decent write-up of your efforts ruffled feathers. How many discussions concerning anthranilic acid are there? Now, if your stated intention is to alter that phenethylamine into another phenethylamine, its Wasp business.

A good extraction/purification is just that, and good practice. Harder than it sounds.

Luck!

*edit* How about weight of starting material, solvent volumes, orders of washing, etc? Keep a LOG BOOK, as it can save your butt. This is through personal experience, and one of our illustrious mods also. To a lot of LE folks, everything is a meth lab. A log book documents intentions, etc. I was at church one Sunday in Nevada, got a call. City Cops wanting to "Know where I was". My house was on the same block, and I walked outside to a street full of cops and fire trucks. Long story short, the Detective and Fire Chief both told me that people keeping notes generally aren't the ones need worried about. The left quickly, and didn't take any of my stuff. Suspicious neighbor called. (I saw a FLASK! OH NO!!!)

[Edited on 10-13-2020 by arkoma]

chemist1243 - 13-10-2020 at 15:52

Quote: Originally posted by arkoma  
The Wasps know how to de-gakk pills, and "thou dost protest too much." Be advised that PPA is a List 1, if it matters.

I would be rather surprised if a decent write-up of your efforts ruffled feathers. How many discussions concerning anthranilic acid are there? Now, if your stated intention is to alter that phenethylamine into another phenethylamine, its Wasp business.

A good extraction/purification is just that, and good practice. Harder than it sounds.

Luck!

*edit* How about weight of starting material, solvent volumes, orders of washing, etc? Keep a LOG BOOK, as it can save your butt. This is through personal experience, and one of our illustrious mods also. To a lot of LE folks, everything is a meth lab. A log book documents intentions, etc. I was at church one Sunday in Nevada, got a call. City Cops wanting to "Know where I was". My house was on the same block, and I walked outside to a street full of cops and fire trucks. Long story short, the Detective and Fire Chief both told me that people keeping notes generally aren't the ones need worried about. The left quickly, and didn't take any of my stuff. Suspicious neighbor called. (I saw a FLASK! OH NO!!!)

[Edited on 10-13-2020 by arkoma]


Yes, extraction is an art. I suck at it and will continue try until i get a grasp. We’ll see what comes of it. If i do manage do get a decent write up, ill post it in publication section.

Ps - i take logs, thanks for asking though. If the police get to me the first thing ill do is call my lawyer. The second thing ill do ask how they didn’t get here sooner. I live in the suburbs for god sake! Eh, who cares, i know they’ve watched me before. I be a “good boy”, keep notes, dispose waste properly, and dont buy too many list one chemicals, pay in cash when possible, and no one goes to jail. simple.


Panache - 13-10-2020 at 23:28

i'm assuming in this context a wasp is not a white angleo saxon protestant, so what are they?

arkoma - 14-10-2020 at 01:12

thevespiary.org


zed - 16-10-2020 at 20:16

Well, it is possible that if you acidified the material with Sulfuric acid, and you steam distilled it, you might be able to isolate Phenyl-2-Propanone from the distillate. Such an approach works on ephedrine.

The Amino-Alcohol is first dehydrated, it then isomerizes to an imine. The imine is hydrated to yield the ketone and Ammonia. Since the solution is acid, the Ammonia is captured as its non-volitile acid salt. While the poorly water soluble Phenyl-2-Propanone is distilled out of the solution.

About a 70% yield as I recall. Now, I probably wouldn't do it, but it's an interesting idea.

morganbw - 17-10-2020 at 05:26

@Zed
Nice post, this has escaped me and I am not young.

arkoma - 17-10-2020 at 07:58

why can't MY dog be prescribed this stuff? *sigh*

How's the project going chemist1234?

karlos³ - 17-10-2020 at 11:08

In my experience, I "prescribed" my dog racemic ephedrine made from the aminoketone and that works wonders.
Not only defeated it her leaking problem, it acts like an antidepressant and had a profound effect on her mood :)
I just wish I could make it into chewable tablets and wouldn't need to weigh every single dose out myself.

chemist1243 - 17-10-2020 at 12:45

Update:

Here’s my lab notes from the attempted extraction:

5 75mg “proin” chewable tablets are crushed into a powder and added to a flask. Methanol is added until the proin is completely submersed, and then the mixture is magnetically stirred(medium) for 1 minute. The light-brown slurry is filtered and the resulting liquid is transferred to a beaker. The wet proin is transferred from the filter paper back into the flask and the extraction is repeated 2 more times with fresh methanol. Then i did one more wash just to be sure. The combined methanol extracts are evaporated on metal pan.

The residue left on the pan after evaporation is taken up in dilute HCl solution(PH of 3-5). I stirred it around for 5 minutes with magnetic stirring to get a cloudy yellow solution and filtered it to get 60ml of a now clear yellow solution. 1.2g(I wasn’t trying to be specific, i just measured out what I thought would be enough to make the solution basic) of KOH is stirred in. I let the solution cool to room temp and then extracted it 3x with 10ml of starting fluid(new starting fluid each time). The combined starting fluid extracts are dried with 3.5g(again, the amount wasn’t based on anything) of oven dried epsom salt. The starter fluid extracts are extracted 3x with 20ml of dilute HCl solution, the organic layer is disposed of, and the acidic extracts are evaporated on a metal pan to yield, quite disappointingly, short green crystals.

Basically, My stupid ass made the mistake of evaporating a mineral acid solution on metal surface, which tainted the “product” green. Either that or there was some kind of green coloring in the tablets, but i doubt the presence of any added colorings. There is also the possibility that there was never any product in the solution to begin with, and the crystals are just a result of the formation of metal salts on the surface of the pan.

Once i get my hands on some more proin ill go ahead and redo the experiment with my previous mistakes in mind.

Before i go do any other extraction methods though, I’m going to perform the EXACT same procedure in my notes but with a glass evaporation dish(no plastic coatings), then ill know for sure if it was the pan that caused the green color.

karlos³ - 17-10-2020 at 12:52

Why haven't you just taken up the freebase in DCM or better ether and precipitated it with acetonic oxalic acid solution?

chemist1243 - 17-10-2020 at 12:55

Quote: Originally posted by zed  
Well, it is possible that if you acidified the material with Sulfuric acid, and you steam distilled it, you might be able to isolate Phenyl-2-Propanone from the distillate. Such an approach works on ephedrine.

The Amino-Alcohol is first dehydrated, it then isomerizes to an imine. The imine is hydrated to yield the ketone and Ammonia. Since the solution is acid, the Ammonia is captured as its non-volitile acid salt. While the poorly water soluble Phenyl-2-Propanone is distilled out of the solution.

About a 70% yield as I recall. Now, I probably wouldn't do it, but it's an interesting idea.


Maybe ill try it out when i get my hands on an ounce or 2 of pure ephedrine or PPA(in my wet-dreams). Until then its sub-10g reactions for me lol ;)

chemist1243 - 17-10-2020 at 13:07

Quote: Originally posted by karlos³  
Why haven't you just taken up the freebase in DCM or better ether and precipitated it with acetonic oxalic acid solution?


Because I’m kind of a huge noob and haven’t even heard of using oxalic acid solution to precipitate amine salts until now. Enlighten me, what are the advantages of precipitating out an oxalate salt from solution as opposed to evaporating an acidic aqueous extract or gassing a non-polar freebase solution with HCl? HCl may be awful to handle, but its basically the “go to” salt for any phenylethylamine and is a notoriously reliable way to salt a freebase amine and precipitate from a solution.



karlos³ - 17-10-2020 at 14:28

Oxalate salts form prefereably well from impure solutions of an amine freebase in an acceptable purity, that can almost be generalised.
Directly after the picrate!

chemist1243 - 17-10-2020 at 16:02

Quote: Originally posted by karlos³  
Oxalate salts form prefereably well from impure solutions of an amine freebase in an acceptable purity, that can almost be generalised.
Directly after the picrate!


Oh, so basically the oxalate salt precipitate from an freebase amine solution is more pure than the HCl salt precipitate from the same solution? I can see how that would be very convenient compared to handling anhydrous HCl gas. I’m assuming 1:2 molar ratio of oxalic acid:freebase works okay, right? Does the concentration of oxalic acid in an acetonic solution matter, or does there only have to be enough acetone to dissolve all the oxalic acid?

zed - 18-10-2020 at 00:52

Well, actually HCl gas is remarkably easy to handle. Just put together a rudimentary apparatus, and drip concentrated H2SO4 onto rock salt. Then, use a hollow glass tube to bubble the gas through your solution. Trap the excess gas, and entrain it with an aspirator pump. Just don't breath it in.

Doesn't mean you want to form a hydrochloride though. If the guys like oxalic acid for the job, I gotta think it's probably the way to go. I've never done such a thing myself.

Oxalic acid is more of a worry than HCl gas. Very poisonous.

[Edited on 18-10-2020 by zed]

arkoma - 18-10-2020 at 05:09

Well, it takes something (balls?) to post a write up of a failure, but as you (AND I) know, extractions have a damn learning curve. Mechanical losses add up quickly also when dealing with small quantities of pills with small amounts of active ingredient each..
Quote:
when i get my hands on an ounce or 2 of pure ephedrine or PPA(in my wet-dreams)
Well, then you would lose the fun, adventure, and practical skills gained by extracting/purifying it yourself......

Hang in there.

Panache - 18-10-2020 at 10:20

Quote: Originally posted by karlos³  
Oxalate salts form prefereably well from impure solutions of an amine freebase in an acceptable purity, that can almost be generalised.
Directly after the picrate!


are you kidding? Wow, omfg!!

chemist1243 - 18-10-2020 at 11:32

Quote: Originally posted by zed  
Well, actually HCl gas is remarkably easy to handle. Just put together a rudimentary apparatus, and drip concentrated H2SO4 onto rock salt. Then, use a hollow glass tube to bubble the gas through your solution. Trap the excess gas, and entrain it with an aspirator pump. Just don't breath it in.

Doesn't mean you want to form a hydrochloride though. If the guys like oxalic acid for the job, I gotta think it's probably the way to go. I've never done such a thing myself.

Oxalic acid is more of a worry than HCl gas. Very poisonous.

[Edited on 18-10-2020 by zed]


Still, I’d rather deal with poisonous solid than a poisonous gas.
HCl is not “remarkably easy to handle”, at least for me.

karlos³ - 18-10-2020 at 13:27

Quote: Originally posted by zed  
Oxalic acid is more of a worry than HCl gas. Very poisonous.

Now that is really an exaggeration.
You can take up to a half gram of oxalic acid daily.

In case of several arylmorpholines which badly form HCl salts but very well oxalates, I have, and others did too, used those substances as oxalates.
A good example would be amphetamine to illustrate how little oxalic acid one actually intakes, I did the math quick and I found that 1g of amphetamine hemioxalate contains only 400mg of oxalic acid, but the dose of the base but would heavily out of question.

So the actual intake of oxalic acid is quite low and one can stand a bit of that stuff.
A strawberry-rhubarb cake probably contains 200mg of oxalic acid per "dose" or rather serving, already.

My dog of course gets the HCl salt, even those minute quantities of oxalic acid aren't that suitable for a small dogs kidneys in such an advanced age, even if we talk about single digit amounts in milligram daily.

Corrosive Joeseph - 31-10-2020 at 10:34

Quote: Originally posted by zed  

Now, I probably wouldn't do it, but it's an interesting idea.


Some bedtime reading for zed....

https://erowid.org/archive/rhodium/chemistry/p2p.ephedrine.h...
https://erowid.org/archive/rhodium/chemistry/phenylacetone.h...



/CJ

zed - 31-10-2020 at 19:39

Ummm. Oxalic Acid is less poisonous, than I imagined. Perhaps, working with Oxalyl Chloride, left me with a negative impression. To me, the Acid Chloride, seemed pretty nasty.

https://occup-med.biomedcentral.com/articles/10.1186/1745-66...

Ingesting a fatal amount of Oxalic acid might require 5 Grams or more. Depending of course, on how crappy you kidneys are to begin with.

[Edited on 1-11-2020 by zed]

karlos³ - 1-11-2020 at 04:32

Believe it or not, simple simple oxalic acid doesn't even fume in the air! :o