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Alternative to purify amphetamine sulfate

Doclad

Bluelighter
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Mar 17, 2015
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Hi.

I've received 3g of amphetamine sulfate that smells slightly of apple and is like a semi-solid paste. I know it is not pure, and I need your help.

So far I have always dissolved the paste in water to discard substances insoluble in water and then I have done a wash of pure acetone to discard solubles in acetone. The purity yields have never been higher than 80%, and of the remaining percentage EnergyControl has not been able to tell me what substance it was. They would call it "Byproducts of synthesis".

I've thought about an a/b extraction, but I usually find that this method leads to a significant loss of performance. High purity, yes, but little performance.... I use NaOH to basify, Toluene to extract, and HCl to salting, but I read somewhere that Amphetamine HCl isn't a good idea.

I was wondering if there is any solvent that is capable of dissolving Amphetamine Sulfate at boiling temperature and is almost insoluble when it is frozen, or if there is some alternative method so that you can obtain a very pure product with good performance.
I've at my disposal methanol, ethanol, hexane, toluene, dichloromethane and acetone.

Thanks


DocLad
 
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The HCl salt is avoided because it tends to be super hygroscopic (absorbs water from the air) but if you work with it in solution it should be fine. The sulfate or phosphate salts are preferable (use sulfuric/phosphoric acid resp. to neutralize the freebase). (see SWGDRUG's monograph)

If by "performance" you mean the yields are poor, using DCM for the acid/base extraction will result in better yields as it is a much better solvent than toluene for amphetamine freebase. And make sure to extract everything 3x.

Washing with cold anhydrous acetone works fine to get most of the impurities off though.
 
I was wondering if there is any solvent that is capable of dissolving Amphetamine Sulfate at boiling temperature and is almost insoluble when it is frozen, or if there is some alternative method so that you can obtain a very pure product with good performance.

Anhydrous IPA will, and is reasonable for recrystallising like that, and should be relatively easy to get and dry, but I can't see any real advantage over a few acetone rinses (and you'd still want to acetone or CWE to get the caffeine out anyway, as that'll tend to form interlinked crystals). Make sure your product is as dry as your solvent too.

Also, fyi, some of the crap in your product probably gives it some of what you consider to be its 'good performance', so cleaning it might be counterproductive from that pov.
 
CFC, what do you mean with crap? I like to take pure substances, it's the only way to test them correctly. If I want to make a mixture, I do it conscientiously, I don't want unknown substances that can "improve the experience" because they could hide other unpleasant effects. This forum is to avoid possible harm to drug users, I think your comment is not very accurate.
Anyway, I'd like to know if you're not worried about taking unknown substances, at least I do.

Sekio, I've noticed some problems with DCM. I've the feeling that water retains much of the DCM inside.
DCM water solubility:
25.6 g / L (15? C)
17.5 g / L (25? C)
15.8 g / L (30? C)
5.2 g / L (60? C)
17.5g/L does not seem very soluble? Would not there be a decent amount of amphetamine base in DCM dissolved in the water? Maybe I'm wrong, but Toluene has a much lower solubility. If this point is not important, I can continue with the extraction a / b without problems. I've 85% phosphoric acid, the problem is that I don't know how much amphetamine-free base it would have, and unfortunately the phosphoric acid will not evaporate.

But now that I think about it ...
I also have fumaric acid! Can I do Fasa by adding the amphetamine base dissolved in DCM drop by drop, as with DMT? And then put the acetone in the freezer to precipitate the crystals? Maybe this is the best solution. I wait your answer.


DocLad
 
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I think your comment is not very accurate.

it's true though, subjectively a mixture of amphetamine and caffeine will seem more "stimulating" than either drug alone.

Sekio, I've noticed some problems with DCM. I've the feeling that water retains much of the DCM inside.

DCM dissolved in water does not have the same solvation power as DCM as a pure liquid. The DCM molecules mixed with water won't be able to solubilize anything very well, but the bulk phase that seperates to the bottom will.

Besides if you are doing the extractions the way you should have been taught in high school chemistry, you'd do at least 3x extractions with small portions of DCM so anything you "misseD" in the 1st extraction will likely be taken up by the 3rd.

If you are lazy then the best thing to do is just wash with cold acetone like I stated earlier.
 
Yes, then in that case they aren't crap, it's caffeine. What I wanted to say is that it is important to know what other substances are in the product. If they can augment the stimulating effect and that is the desire of the consumer it seems good to me, but I don't think we should ignore what it is about.
I'm sorry if I don't explain myself better about the importance of knowing what we are taking, whatever it may be.

I understand what you want to say about DCM, I will certainly use it ahead of Toluene.

Regarding the fumaric acid ... do you think it is possible to salt the amphetamine base in acetone saturated with fumaric? I tried this process with 3-mmc but it never crystallized.


DocLad
 
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Depending on the route of synthesis and conditions used the crap may be other amines (e.g. bis(1-phenylpropan-2-yl)amine) which will forms salts just like amphetamine does, these side products you can't get rid of using acid/base extraction and they add to the weight of recovered material.
 
Hi Sumador.

I had thought that too. In that case, what options are there to separate amphetamine from those other compounds that wouldn't be separated with an a/b extraction?


DocLad
 
That's a rhetorical question, Sekio? 8)

Here the expert is you.


DocLad
 
Alternatively, distillation of the freebase under reduced pressure is a another option considering the difference in molecular weight but that would require a reasonably high amount to have to start with, otherwise you would inevitably lose a lot of material, or a specialistic apparatus for short-path distillation of smaller amounts under reduced pressure (Kugelrohr). Selective recrystallization of amphetamine should be possible with the right acid and solvent(s) used, but without a ready protocol working in the blind is pointless IMO if you can't then check what crystallized out. Preparative liquid chromatography is an obvious choice, but that's a different story, it has one big downside, you usually need relatively large volumes of solvents even for small samples unless your desired compound can be selectively washed out of a small amount of an adsorbent with the impurities staying behind adsorbed or the other way around. Solvents then of course may be recovered but if you use a mixture of solvents as eluent which is very often the case, certain azeotropic mixtures will not be possible to separate into pure solvents.
 
From Dutch data it appears that most clandestine amphetamine is in the form of the sulfate addition salt. From the GC-MS it is clear that the Leuckart reaction is the preferred route. Even the sulfate is hygroscopic so what HR agencies term 'base' is still only 50% pure because it is cut immediately to avoid ending up with a rather caustic gel. This isn't to say other routes aren't used, just that the large-scale organized criminals go down that pathway. It makes sense. Almost nobody who is discovered making it has a formal education so the simplest way to 'cook' a product will be attractive because of the small skill-set involved.

I have witnesses people suffering from stimulant psychosis and it can be very scary. In the UK we have x4 more people using IV amphetamine than IV opioids but as a group, they don't come to the notice of law enforcement as often. To health services, yes, but not the police or the ambulance service.
 
Goodnight.

I'm going to deviate a bit from the last comments to ask you a question.

Finally it seems that I have amphetamine sulfate.
Well, my question is a bit general. I read that to purify MDMA can be dissolved in a minimum of boiling IPA and then let cool little by little to grow beautiful crystals.
Does this apply to all amphetamine salts or MDMA only for some reason?
Would this process work with my amphetamine?


DocLad
 
Yes, you can do amphetamine sulfate recrystallization from boiling IPA, but that doesn't present any advantage over acid/base extraction as a method of purification in my opinion (well, other than perhaps having crystal product and not aqueous solution of amphetamine salt in the end which you have to evaporate).
 
Well, the advantage is that heating IPA is cheaper than doing an A/B extraction and it takes less time.
Why would not methanol or ethanol work the same as IPA?
Is there something in their chemical structure that makes them different in that sense?


DocLad
 
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