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

[WillD]

The reaction with sodium borohydride may get out of control if you do not monitor the temperature. In addition, small-dispersed copper compounds can interfere with the purification of the final product.

 

[V€ctor Company]

If
the reaction of the sodium borohydride does go out of control, what can I do about it, is the synthesis botched? If there are small dispersed copper compounds, is it impossible for me to remove them when purifying?

 

[InLikeFlynn]

I had p2np flare up after an unintentional quick addition with the nabh4 it didn’t do anything negative to my final product.

I filter all the copper compounds out with 2-3 coffee filters after letting it sit after the 80c heating.

 

[WillD]

click. Steps 1-5 are better in waterless conditions (with one equivalent of NaBH4). After, with the resulting nitropropane and metal chloride as catalyst, water conditions are possible.

 

[MisterAnonymous]

@William Dampier what is the BP of Amphetamine Freebase and does it need to be distilled under vacuum?
Or does steam distillation also work?
I just want my Freebase colorless like water!

 

[mithyl2]

in the video novator says that around half of the 26.25g CuCl2 solution will be enough to 'cease' the black copper oxide formation.

does he actually use all of the CuCl2 solution, or only half of it?

(the last synth i did i added the CuCl2 solution in an unmeasured amount until the black copper oxide forms at the bottom of the reaction mix. i have yet to determine the quality and yield of the final product).

 

[InLikeFlynn]

Whatever you do, do it on a mg or gram scale first just so you can see what’s going on. That’s a lot of product to waste if you mess up somewhere.

 

[mithyl2]

yes. i've been doing less than 10g batches. will probably go back to 5g until this problem is sorted out

 

[InLikeFlynn]

I’ve been doing 5g batches every couple of months since last year and I’m just now starting to get some good results.

some tips I have is at a small scale like that. Wait into you’ve added the p2np all the way and then heat it up manually to 60c for 30-45 min and the same with the CuCl2 after you’ve added all of it. Heat it back up to 80c and hold it for 30-45.

the video takes a while to add the P2np ans CuCl2 due to bigger synthesis, but at lower quantities it is kinda needed to get the reductions going.

also use as dry as possible of IPA and Acetone, this really has a huge effect on everything, I’ve found.

 

[mithyl2]

I always appreciate tips from real experience. I haven't tried dry IPA yet

what is your source of p2np?

 

[InLikeFlynn]

Found it on eBay. Currently in the process of teaching myself how to make it.

 

[mithyl2]

has anyone else had a much larger amount of substance precipitate at the last step?

after i did the precipitation step with phosphoric acid i had more than 4 times the amount of what should be amphetamine precipitating

 

[Gordon Ramsay]

Very interesting, I'll observe and wait for an explenation of the experts on this I have heared typical street rumors as to the fact that phosphoric acid is supposed to increase yield but I'd wonder why it would yield more and also what effect this would have on the purity of the product. Amphetamines from phosphroic acid are supposed to be a little weaker, aren't they?

 

[Gordon Ramsay]

As far as I am informed it is doen within the same synthesis as for Nitroethane but it is done with Nitromethane.
The smell, apperance is the same but there are no amines.

I think it is called Nitrostyrene but I am not sure if I remember it correctly

Edir: It is called B-Nitrostyrene

 

[mithyl2]

can you say what's the best way to check if i have genuine p2np?

 

[GhostChemist]

It`s not necessary to evaporate IPA, but the T of mixture must be raised to 60C.
If the all chemistry is pure, that possible too much of CuCl2 could have reacted with amine.
Can you describe the colour of the mixture when adding CuCl2?

 

[Gordon Ramsay]

You can carry out a Melting point determination

MP P2NP 64-66 °C
MP B-Nitrostyrene 58 °C

Melting point can vary due to product quality of course, it will be most accurate when the product is perfectly pure..in case your product quality might be low, you could recrystalize and then carry out a MPD!

 

[mithyl2]

the moment i added the copper solution (i used CuSO4*5H2O) to the rm it turned dark grey. i added it slowly, and after the first few drops i turned on the heat. (there was also what looked like undissolved borohydride granules in the rm.)
as i continued to add it it didn't really change color, but the copper oxide sediment formed like in the video. because of my hotplate i couldn't get the temp above 62C, so i kept it at 62c for about 3 1/2 hours.
However, i did another synthesis where there weren't any granules in the rm, and i held the temp at 80c after the addition of the CuSO4*5H2O solution, and it still gave the same product at the very last stage.

there was a synth i did where the rm turned dark green upon addition of CuSO4*5H2O, and after a few more drops it turned dark orange.

with all the synths i've done, everything in this first stage has at least appeared to be consistent with the video.

i think with all the synths i've done so far, after the addition of the CuSO4*5H2O i have either left the rm as is with the copper oxide sitting at the bottom for a couple of days before i separate it, or i left the separated solutions with the 25% naoh solution in them sitting for 2 days. could this be a problem?

also something strange that happened was something precipitated in the 'main orange solution' after leaving it for a couple of days on it's own, whether it was left with the naoh solution after seperation, or just left for 2 days before seperation with the copper oxide at the bottom. (i don't think the solution derived from the copper oxide extraction had any precipitate).

maybe another potential problem is that when i recrystallized some my p2np i tried using sodium bicarbonate to purify it but i added too much (about the same amount of sodium bicarbonate as p2np. i added it in solution when the p2np was dissolved in a hot etoh solution. (i then put it in the freezer, filtered it when the p2np had precipitated, then did a standard re-crystallization by just dissolving it and precipitating it after freezing.) but maybe the sodium bicarbonate wasn't removed. a possibility is that maybe the sodium bicarbonate is present in the p2np i'm using.

 

[mithyl2]

thanks gordon.

i did i think 3 recrystalizations, so i should have a very pure product. at this point it has a fluffy consistency, has a faint smell, where it was once very pungent, and is a light yellow color.

 

[GhostChemist]

In this step, it`s probably to leave RM for 2 days is a mistake

 

[mithyl2]

i'll try and do it in one run. is there anything else i did that you could say might be the reason for my apparent failure?

is CuSO4*5H2O definitely ok to use instead of CuCl2?

i will post a picture of my p2np soon. hopefully tomorrow.

 

[GhostChemist]

CuCl2 is more soluble than CuSO4*5H2O, which may lead to dilution of RM.
Sometimes, after adding CuCl2 and NaOH the RM can solidify after 20-40 min and the solution of amine can be easily decanted.

 

[mithyl2]

i noticed this. in one batch i did i added a little more water to the CuSO4*5H2O to make sure it all dissolved. but it wasn't dissolving readily. can you say how much extra water could be added before it's a problem?

 

[GhostChemist]

As a variant proportionally decrease the volume of water in the NaOH solution

 

[EileiterBurner]

In the evening I did a few experiments again today, I used methanol instead of IPA.

What I can say is that 2 layers don't form when you add NaOH.

Which I don't think is a bad thing in this case, because you can immediately precipitate the salt...

And what I can also say is that the speed is very strong in the turn and I haven't had such quality in a very long time...


PS.sorry for my bad englisch

 

[PabloEscobar]

Thank you for the synthesis & video GhostChemist. I have one question: Has anyone calculated the purity of the final product?

 

[GhostChemist]

The chemical analysis show that the Na2SO4 is presence as an impurity when alcohols were used. In most cases, the purity depends on the starting reagents and further purification.