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

[ACAB]

Water alone does not lower pH, only acid does.
No you can't just raise the pH again to get freebase, you have to first filter the salt, dry it, then dissolve it in water and then you can raise the pH again to get freebase.
Basically you should work with very dry liquids if you want to salt out something, because as we know salt always dissolves in water, thus any water content is bad for yield. If your acid contains 15% water, 0.75ml of water in 5ml acid can give you less yield, plus the water that is still in the acetone. Cooling the solutions makes sense because the solubility decreases with the temperature and therefore the yield increases. It is best to dry the solution with MgSO4 in the freezer.
If you add acetone to the freebase/IPA you can counteract the effect of too much solvent, more salt precipitates again, at least this is the case with sulfate.
You can also let the solvent evaporate, but you should not use too much heat for this.
~200°C, but the freebase would decompose before that. I was told not to make freebase warmer than 60°C, otherwise yield lost.

 

[Montecristo]

thanks for that. yeah i was meaning the water in the acid and solvents rather than water alone, i didnt dry anything. I just checked the freezer and i have a thick layer of precipitate at the bottom which is great to see. In the future ill aim for higher yields by following drying methods etc, and will probably use sulfuric. This run i just needed money as soon as my NaBH4 came through.
Thankfully i didnt exceed 60C when i evaporated solvent off, but its good i know that now.
I will get back to you guys with my yields and maybe document my next run .
All in all this synthesis was fun, very simple and effective. i can do 70g P2NP in a 2L flask which is much better that the Al/Hg method @ 10g. I will give the Al/hg method a go sometime though , just for fun.

 

[Montecristo]

I yielded 40% white (ever so slight grey tint), bone dry phosphate salt.
This was from my brown P2NP and i def lost some freebase to not knowing the main extraction was in the top layer.
I am very happy for a first synth, despite yield being low.
With more cleaning of P2NP and if i implement drying protocols, i should be on my way to a higher yield.
Thank you everyone who helped me along the way, I will continue to play around with it and when i am happy with yields i will write up the method for other amateurs.
Cheers!

 

[ACAB]

if this precipitate falls out before add acid filter it off before add acid.
You can dry all solvents in the process before adding acid with MgSO4 (or other drying agents) in freezer and filter it off again
The salts of sulfuric acid and hydrochloric acid are some of the most stable compounds, I believe sulfate has the highest yield, which is why it has become popular.
For this reason, only vacuum steam distillation is recommended for cleaning the freebase, if it is to be carried out.
With me it is exactly the other way around I only know the Al/Hg variant, but I recognize the advantages of this method and will try this one as well. Results I will also present here, but that will still take a while, first I have to improve the Al/Hg method, but I think I'm on a good path.
You have to recrystallization in hot IPA, or water P2NP must be just yellow. If your P2NP has turned brown, it is oxidized and no longer usable, store it in an airtight container in a cool (<8°C) and dark place, such as the refrigerator.
Not only if you had good results this can be helpful for beginners, also bad results can be discussed here, I did and you get a lot of advice that may help you further. That's the whole point, perfect syntheses we have in the manual. Good results can of course also be presented to pick up the pats on the back

 

[Montecristo]

i filtered the precipitate after basifying.
Ive had alot more precipitate , acetone used to wash was placed into the orginal alcohol acetone mix and placed back into freezer.
My yeilds looking like 50+% at the moment and hopefully more comes after a night in freezer.
I tried 25mg of it and it is very strong, the stuff im used to is likely about 75% cut.
Sometimes you just have to do it yourself

 

[Montecristo]

I will write up what i did differently tomorrow.

 

[Montecristo]

The P2NP was dark brown , i did 2 ipa recrystalisations and got clear ish crystals with a brown tint, i think it was as good as i could get it without wasting too much time, but now i have some product i will keep washing until IPA is clear. I think next time i will make it myself and store it properly.
Thanks for the advice!

 

[Montecristo]

i have now reached 60%

 

[Montecristo]

Here was what i did on a smaller scale;
1. Solution IPA/H2O 2:1 ((IPA 800ml,H2O 400ml)(1200ml)) was added a 2000ml flask.
2. NaBH4 (116 g) was added at once and stirring was started.
3. P2NP (67 g) was added in small portions, so that the temperature of the mixture did not exceed 60 *С.
4. CuCl2 (7 g) in water (13 ml) was added slow dropwise, so that the temperature of the mixture did not exceed 80 *С.
5. Thereafter, reaction was refluxed at 80 °C for 30 minutes using external heating.
6. Solution is decanted and filtered from reaction waste and put into a seperatory funnel.
7. 25% water solution of NaOH (533ml) was added to reaction mixture and the phases were separated.
8. Drain the bottom layer into a large beaker and collect the top organic layer.
9. The aqueous phase was then put into the seperatory funnel and extracted with 500ml of IPA.
10.IPA was evaporated by 3/4, half milky freebase and half IPA.
11.The IPA and freebase was dissolved in 130ml of acetone.
12.orthophosphoric acid dripped to pH - 6 (with constant stirring).
13.The mixture was put in the freezer for 12 hours.
14.After crystallisation the suspension was filtered and washed with dry cold acetone, until acetone is clean.
15.Acetone from washing and the ipa/acetone mix is placed back into freezer for further precipitation.
16.Process repeated until no more precipitate to yield 60-70% high quality amphetamine, as the mix gets more acetone in it you may need to drip some more acid to bring it down, but not too much as acetone is ph7.

Here is a photo of some of the dried paste rocks , the rest is dry powder to be mixed, as it is too strong for me and my friends.
I may update the recipe and do a write up for the small scale home chemist, there are lots of ways this could be better.

 

[flyhigh]

this is no meth , can you write from here on how to make it to crystal meth

 

[Amin. M]

What method do you use to convert this white paste into crystal
d-methamphetamine?

 

[ACAB]

Before consuming I would still clean it, it looks quite dark in the photo from yellow to brown.
But congratulations on the successful synthesis.

 

[Honolulu98]

Where did you buy the crystal rector?

Directly from China? Did you have any problems?

 

[btcboss2022]

From China but using a company that is used to order this kind of equipment, anyway for equipment normally shouldn't have any problem, for products is different.
For equipment supplier can make docs and invoice with any other equipment name if you apply it for sure.

 

[Sasha89]

Hey guys!
At what speed are you stirring during the synthesis and is it a constant stirring?

 

[Mystery_chemistry]

hello everyone, please help, can there be a problem with the pH reading after adding 25% NaOh solution and extracting the water phase of IPA?can I extract a dxm aqueous solution instead of IPA?

 

[Mclssmxxl]

I’m not sure what you mean but you should extract the water phase a couple of times with a non polar solvent like toluene,petroleum ether

 

[Mystery_chemistry]

and what do you think about adding AcoH after the reaction is finished? in some recipes they write about adding ...

 

[Mystery_chemistry]

Ok I understand . as a last resort, it can also be dcm as handy?

 

[Mystery_chemistry]

I have a question. if I do a dcm extraction, so as not to play with distillation, can I perform an acid-base extraction? two phases should form when acid is added to the freebase in dcm. at the top, the product at the bottom, muck. separate, add alkali to product to obtain ph12. there should be a pure oil (freebase), separate from the bottom layer and dry with sodium sulphate. head well or bad? please help

 

[ACAB]

With petroleum ether you do not extract an aqueous phase, petroleum ether and water do not mix.

 

[Mclssmxxl]

I have extracted numerous times with petroleum ether but maybe I’m dumb..