One-pot Amphetamine Synthesis From P2NP With NaBH4/CuCl2 (1kg scale)

[Uncle Lee]

This reaction is very good on a small scale
In a large reaction, trying to control the exotherm and the large amount of foam by putting the CuCl2 solution slowly into the flask will not give a high yield, there may be nothing but nitroalkanes and the concentration of nanoparticles will be too small to reduce the nitro, the largest flask possible should be used and the entire CuCl2 solution should be added at once

 

[RickyKasso]

What do you consider as "small scale"? Is there any specific amount of P2NP and respective amounts of the other chemicals to have the most optimal and easy going reaction?

 

[UWe9o12jkied91d]

30g

 

[aa1178251182]

 

[aa1178251182]

This kind of reactor is very suitable for this reaction

 

[AKWA]

Yes. I figured with all the mandarin texts all over but a more specific route, Idek what they're called or the site.

 

[UWe9o12jkied91d]

there's 4 glass manufacturers on aliexpress where you can buy directly or talk to a reputed vendor on alibaba

 

[spikkel]

About the amphetamine synthesis, part from amphetamine base ( A-oil ) to amphetamine sulphate. Normally we use a mixture of sulphuric Acid and acetone to add to thé base so we het sulphate. Now in my country/region everybody uses methanol instead of acetone and sometimes even mix thé A-oil with methanol for making thé "Belgium/ditch" amphetamine "paste' so i was wondering if it's possible for thé methanol being replace with bio-ethanol ?

 

[blackburn]

You can use methanol, IPA , aceton. Bio ethanol should be fine...

 

[spikkel]

tested and succeeded, frankly better than with methanol (gives a softer taste to the end product) and it is cheaper and freely available in shops or on the internet (with a purity of 96 - 100%). again discovered/learned something in this magical place, thanks guys

 

[w2x3f5]

It is interesting to try this synthesis, but modified. The yield of 70 percent is most likely due to the fact that have to reduce the nitro compound in an alkaline environment, because of this, the yield of the amine and impurities is the incomplete reduction of the nitro compound. Only in an acidic environment will the reaction equilibrium shift towards the formation of an amine, an example of this is the reduction on amalgam.
Copper nanoparticles can be obtained separately, a mixture of copper chloride in water and a reducing agent, iron or hydrazine.

 

[Melv99]

Do you mean it shirts to an amine at the same step during titration? Or sometime during the process? Just curious

 

[w2x3f5]

this synthesis is two-stage. the first stage is the reduction of the double bond in nitropropene with borohydride. the second stage is the reduction of the nitro group on a copper catalyst, borohydride is only a source of hydrogen for the copper catalyst, therefore, it is possible to change the reaction and carry out reduction in an acidic environment, the reducing agent can be changed. By reducing in an acidic environment, it is possible to increase the yield

 

[SelfExper1menter]

Hello everyone. I tried to make some amphetamine using this recipe on a small scale, but failed. Everything seemed ok, after drying my product looked like white powder with a tinge of redness. If it was amphetamine sulfate (which I was trying to make), the yield would be 84%. The problem is, it's not amphetamine.

Physiological effects
I tried 20-30 mg, there was definitely stimulation, but also it caused fever and, apparently, a decline in immunity: both times I took it for several days in a row, I fell ill with respiratory infections (first time I thought it was a coincidence). Another person that took it did not experience any stimulation from up to 90 mg, only some mouth dryness. Neither of us have any tolerance to stimulants.

Chemical testing
1 g of the powder completely dissolves in 10 ml H2O.
When I added excess NaOH solution to a measured mass of the powder in a test tube, I got an approximately right volume of freebase smelling of ammonia. I separated the freebase layer, dried it with CaCl2 and tried to titrate it with acid. As a result, I measured molar mass of the freebase to be about 171 (and for amphetamine it's 135). While my measurements weren't very precise, the difference is still too large to be explained by measurement errors alone.

My deviations from the procedure
1) When adding P2NP, I realized it was going to take hours, so I got impatient and immersed the reaction flask in a room temperature water bath. After that I was able to add P2NP almost all at once, and the temperature of the mixture didn't exceed 40-50 °С.
2) I was following the video, so I didn't evaporate the IPA and added conc. sulfuric acid to the IPA/freebase layer directly.
3) I didn't have any acetone at the moment, so I didn't add it before acidifying and I washed the filtered "amphetamine sulfate" paste with IPA.
4) IPA is less volatile than acetone, so I had to put my precipitate in an oven for several hours to dry it to constant weight. The temperature in the oven didn't exceed 80 °С.

So, the big question is, where did it go wrong? I wouldn't be surprised with low yield or no product at all, but getting a good yield of an amine that's not amphetamine?!

 

[w2x3f5]

CaCl2 can't use with amine
1.in the first stage, nitropropene is reduced to nitropropane
2.received impurities of various salts in the composition of amphetamine paste

 

[SelfExper1menter]

Could you elaborate a little, please?

Why CaCl2 can't be used with amine?
1. Isn't reduction of nitropropene to nitropropane what's supposed to happen during the addition of P2NP?
2. I know I got some inorganic salts in my product (sodium sulfate or borate), but they aren't toxic and they wouldn't affect molar mass measurement (they just stay in the aqueous layer when I basify out the freebase).

By the way, I tried to purify my product by acid-base extraction followed by steam distillation of the freebase. It still had immunosuppressive effect and the molar weight was too big again. This probably means my toxic impurity is an amine, too.

 

[w2x3f5]

Calcium chloride reacts with amines, see the guide for which desiccants are acceptable to use with amines.
I said that your borohydride first reduces the double bond in propene to propane, and then the nitro group is reduced to an amine on a copper catalyst (I think with impurities of intermediate reduction products, since the reaction of the medium is not acidic due to the use of sodium brhydride).
Of course, I don’t know how real the formation of any organic boranes is in this reaction, but I would boil your powder in acid just in case and then do acid-base extraction.
Do you think copper salts are not toxic? I would clean it of impurities for my own peace of mind.
How did you determine the molar mass, please tell us in detail.

 

[SelfExper1menter]

Determining molar mass: I put 0.55 g of the freebase (dried with CaCl2) in a flask, added about 10 ml H20 and a tiny grain of Methyl Orange (~1mg). Mixed it all thoroughly. At this point I had a slightly orange aqueous layer and more intensely orange freebase on top of it (Methyl Orange seems to prefer freebase). I started gradually adding 3.67% sulfuric acid with stirring. After adding 4.30 g of the acid, the freebase layer was gone, but the solution was still orange. I added one more drop of the acid (total 4.33 g added) and stirred, the solution turned red (which means pH < 4). Thus 0.55 g freebase is neutralized by 4.30-4.33 g of 3.67% H2SO4. Molar mass is therefore between 0.55 / (4.33 * 0.0367 / 98.078 * 2) = 169.7 and 0.55 / (4.30 * 0.0367 / 98.078 * 2) = 170.9 g/mol

 

[SelfExper1menter]

Copper salts would be completely removed by a/b extraction and steam distillation, and my immunosuppressant toxin wasn't. Do you think organic boron compounds could survive steam distillation?

 

[SelfExper1menter]

I wonder, when I dried amphetamine sulfate from IPA in the oven, could amphetamine react with IPA through a nucleophilic substitution, forming something like N-isopropylamphetamine or N,N-diisopropylamphetamine? These would be difficult to separate from amphetamine.

 

[w2x3f5]

But CaCl2 and you need to use a distilled amine, even more fractionally distilled

 

[w2x3f5]

ok, for inorganic substances, if you did acid-base extraction and steam distillation, the question is closed. Yes, organic boron, as far as I remember, happens after a reduction reaction on borohydride, it usually pops up during NMR. But with regard to the reduction of p2pn, I can’t say anything for sure.

 

[w2x3f5]

read police forensic analyzes of amephtamine, but did not see n-isopropyl, maximum acetyl or formyl derivatives. you can search on the Internet, double-check my information

 

[SelfExper1menter]

Well, that was just a hypothesis.

What is the problem with CaCl2 and amphetamine? What reaction happens, exactly? I can't find the guide you mentioned.

Fractional distillation under vacuum is not really an option for me. Even flash chromatography is easier. Plus, I don't think many people (probably nobody) in this thread fractionally distilled their product, yet no one is complaining of getting sick.

 

[w2x3f5]

I hope Google hasn’t completely banned you in the search engine, try looking for complex salts of calcium and ammonia or amine.
It is likely that other users do not have such problems with the substance as you do. You are offered ways to solve the problem, it's up to you to do or not to do.

 

[poe]

Did you get your answer? I am interested in knowing what went wrong also.

 

[cannedgoods77]

yeah , Im interested too , I hope you will get your answer soon , because your deviations , don’t sound too bad