Amphetamine from P2NP via Borohydride+Copper complex 2022 - questions

[mithyl2]

I found this over on dread and apparently the op from dread got it from here. But I couldn't find this exact method on these forums. (There are similar ones such as William Dampiers' 'one pot 1kg synth' which seems practically the same.)

Could any experienced chemists chip in and tell me if there could be any toxic fumes or serious safety concerns involved with this method:


Original extract:

Amphetamine from P2NP via Borohydride+Copper complex 2022 Updated Procedure

This somewhat newly discovered method is one of the greatest achievements of the clandestine chemistry underworld. Also it is one of the simplest and relatively newbie friendly reactions that exist for making drugs. It does not require any very toxic chemicals like mercury salts. It is fairly forgiving, very high yielding, and works very well even at <1 gram scale.

I have seen some mention of this method here on the darknet, What I have NOT seen is any authorship credits or references. If you are not providing references, you are not really doing science. Continuity of collaboration is essential.

The amazing applications of Borohydride and Transition Metal complexes have appeared as early in 1990 in one Korean journal publication. Some mentions of using Copper metal instead of Mercury popped up on some forums, but finally a very very long colloborative thread formed on a well known English language drug chemistry forum and on a well known Russian language forum. If you would like to trace the footsteps back to the original content, you can figure it out very easily by reading this sub's welcome post.

A chemist known as Testex started this method for amphetamine. Much credit is owed to a chemist known simply as Carl on various sites for making this method blossom. The quoted procedure is credited to Fastbreak, another contemporary.

Required background:


Although this is a very newb friendly procedure, you will not be able to just read this write up and reproduce the results without some VERY basic familiarity with chemistry procedure. The write up assumed you are comfortable with:

* Basic chemistry lab techniques and terminology. You should know metric weights and measures. You should now and understand molar weights, molar ratios, and know how to do your own calculations when reading published procedures that only provide molar amounts

* Basic drug chemistry lab skills and knowledge such as solvent washing, liquid-liquid extraction, acid-base extraction, simple distillation, recrystallization, reagent and melting point analysis

* The resources to obtain the required precursor P2NP, the required reagents, Sodium Borohydride aka NaBH4 and Copper Sulfate aka CuSO4.

*The resources to obtain the required solvents and acid/base reagents including ethanol or isopropanol, distilled water, food grade sulfuric acid aka H2SO4, food/lab grade lye aka sodium hydroxide aka NaOH

*The minimum lab equipment. You will need a hotplate+magnetic stirrer, a reaction vessel, proper lab glassware for preparation and purification, scientific grade thermometers, and highly highly recommended to have a distillation kit for the purpose of reflux during the reaction and simple steam distillation for recovering the purified amphetamine when complete.

*It is possible to do this without distillation equipment but only on a small scale and you are risking the health of anyone that consumes the final product. Also the reaction is much more likely to fail or get out of control. Get a distillation set up.

Procedure:

(direct quote from original)


P2NP cas number needed: 705-60-2



80g EtOH 96% (1%MEK) that's ~100ml
40g H2O
5.2g NaBH4
was combined.

then under strong stirring was added 10g of P2NP(grinded into fine powder) in small portions.

after that the mixture was let stirring for 40 min.

then this was heated to 65°C and another 5g NaBH4 was added, followed by 1.5g CuSO4*5H2O (grinded into fine powder).
resulted in bubbling, reflux condensor attached and let it stirred for 15 min until the bubbling stopped, then the mixture was refluxed for 30 min.

after cooling, 47g of HCl (31%) added together with tap water to fill the flask up.

EtOH distilled out.

cooled, made basic with 20g NaOH in ~50ml H2O.

Steam distilled the amine out. Neutralized with H2SO4 and evoporated.

the product was so white that i decided to not wash the powder.

Yield.: exactly 10g Amphetamine sulfate 88.56%



Important Notes:



Special note:Although the author specifically states ‘tap water’ in the procedure, this is a semi-sarcastic meta-jab wrapped inside of layers and layers of inside jokes. Just use distilled water, please. Thank you /u/socat2me


The main point of failure for this method will be the purity of your P2NP. Whether you have purchased it or made it yourself, countless failures were reported over the years and in nearly all cases the cause was insufficiently pure P2NP crystals. 2 or 3 recrystallizations of the yellow crystals are highly recommended.

The reason for the ethanol+MEK mentioned by the author was because this is sold at most drug stores as non-isopropyl rubbing alcohol. However isopropyl alcohol is also an excellent choice of co-solvent.

The ~ 6X molar excess of borohydride is essential for this unique reaction.

The non-recomended alternative to a lab water-cooled condenser for both the reflux during the actual reaction, as well as the steam distillation during the A/B extraction afterwards can be replaced with a tall necked reaction vessel perhaps with a fan blowing at the neck for a 'poor man's reflux', and then a simple A/B solvent extraction instead of steam distilling the amphetamine base. CAUTION it is very very important to completely remove all traces of the copper complex from anything that will be ingested by humans. Distillation is the perfect solution for this, but a thorough solvent extraction with a strong knowledge and experience with liquid-liquid extraction is a possible alternative. You have been warned.

Advanced:


This same system can also be used on similar, or analogous precursors. There are reports of Fluoroamphetamine, MDA/MDP2P, 2C-X, Pseudoephedrine, TMA, and other drugs and precursors successfully made via this reagent system.

Let us close the history books for mercury salt reductions once and for all!

 

[user123qwe]

+1

 

[mithyl2]

could any of the pros like Patton or Dampier chip in and elaborate on this method, and let us know of any health risks that may be involved with the synthesis?
@G.Patton
@William Dampier

 

[G.Patton]

Just be careful with NaBH4 and water. A reaction between them produces a lot of heat and gas, take it into account. You have to keep reaction flask open with reflux condenser. Also, use well ventilated working place and don't use open fire next to this reaction by reason that H2 is evolved.

 

[mithyl2]

Thanks Patton.

Do you think a 30 inch balloon attached to the top of the reflux condenser is enough to contain the gas for a synth as small as the one described in this method? and how toxic is this gas?

 

[G.Patton]

Not too much, you breath by mixture of gases with hydrogen =) Don't use any balloons. It is dangerous because you can blow up with a high H2 concentration and a sparkle.

 

[mithyl2]

what can i do to manage the h2 that evolves from the condenser in a setting such as a bathroom? if i get an extraction fan and duct to extract it, maybe the h2 could spark inside the fan due to it being electrical and producing some heat. i don't have the ability to do it outside at the moment either.

 

[workworkwork]

Maybe put a hose from the condenser to the air outlet with a strong fan. So if there is an explosion as there is so little hydrogen in the air, the explosion will not cause damage.
I'm thinking by myself, not sure if what I'm saying is correct or not.

 

[mithyl2]

could anyone say if this method yields levoamphetamine or dextroamphetamine?

 

[UWe9o12jkied91d]

racemic

 

[diogenes]

This is essentially the same method as in the original post using CuCl2. Can any of the pros comment whether CuSO4 is inferior or identical (equally effective) in this reduction? thank you

 

[mithyl2]

thanks. after i posted the question i realized it must be racemic. then i would have to isolate the dextroamphetamine isomer to get just pure D-amph.

 

[UWe9o12jkied91d]

Yep, keep in mind it’s possible to use other acids than D-tartaric.I have researched this and can tell you more about it if you need elp.cheers

 

[mithyl2]

yes please. pm me if you like.

 

[mithyl2]

could anyone tell me if using 35-36% HCL instead of 31% HCL is ok?

 

[mithyl2]

i'm preparing to do this synthesis but i'm still worried about the sodium Borohydride.

any help would be appreciated:
isn't it dangerous to add it to the flask with 40g H2O?

and what can i do to mitigate the risk of exposing the sodium Borohydride to the moisture in the air while i open a container of it and add it to the solution?

 

[UWe9o12jkied91d]

Mate, you are worried about residual moisture in the air when you are about to expose the compound to pure moisture
Sodium borohydride is non-pyrophoric and widely used in industry especially in Europe and USA, while other compounds are preferred in Asia.In any case in this book I read a certain person worked at a plant where he personally saw operators dumping 25kg bags of the stuff into the bunker of a 12 ton reactor followed by an addition of the entire contents of the bunker over a few minutes into alcoholic aq. sol, this is routine, you don't have anything to worry about, just watch the eyes and tender bits.Skin contact is also not a big deal discounting the toxicity, in the same book I've read operators would get their hands contaminated and all would happen was temporary lightening of the skin and a bit of a burn that would go away with washing.
If you want to be super safe you can add the borohydride under stirring with the flask in a cooling bath, removing it to add propene, then cooling only if needed.You can do this addition over 30s-1m or so with a solids funnel, slowly pouring it in at a constant rate.
There is not going to be an explosion you deliberately take a lighter to the top of your condenser.Given appropriate ventilation you are not in much danger.

 

[mithyl2]

ha, i guess i'm being too paranoid.

what kind of ventilation would be adequate? is the h2 being directed out of an open window with a ptfe pipe enough?

 

[UWe9o12jkied91d]

it's overkill, but depends on scale
fans and open windows or maybe a diy fume hook is plenty for small to medium scale

 

[mithyl2]

i've finally got round to doing this synth and i'm on the very second to final step of steam distillation, but i'm having a problem:
how do i know when all of the amine has finished steam distilling from the flask with the mother solution to the collection flask?

notes:
-solution was very dark orange before distillation began. (solution takes up about 3/4 of the flask).
-to begin with the solution in the collection flask is a clear dull-goldenish color
-after about 1 1/2 hours the solution is the same color, but i think there appeared to be 2 layers (the golden color layer on top, and i think a transparent with a cloudy almost substance consistency in it on the bottom layer.) - (perhaps this is my answer)
-i had to decant this solution in the collection flask because this flask was too small, and i noticed that in the second round of distillation was cloudy white, not orange. (like cloudy lemonade color)