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One-pot synthesis of amphetamine from P2NP with NaBH4/CuCl2 (1kg scale)

btcboss2022

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i didnt get much salt precipitate out when i added phosphoric acid on my 67g p2np batch.
will this change during freeze? i thought i had followed instructions pretty well.
after p2np addition is complete do you go straight to cucl? or should i wait for it to stop reacting?
i shook it up after adding the lye and left it for about an hour, and when extracting with ipa i let it separate and then mixed again 3/4 times.
i vacuum distilled off the ipa @ 50-60oC , was this too hot?
maybe i acidified it too quick, as my sep funeel still had the aqueous layer ( i am doing 2 ipa extractions just in case) so i used a syringe and it wasnt dropwise exactly..
any ideas? i will update after its been in freezer overnight
Phosphoric acid? Where you read that?
 

Montecristo

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hold on is the organic phase after basifiying loaded with product? is it just the IPA from step 1?
 

G.Patton

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orthophosphoric acid yeilds amphetamine phosphate, which i what i was going for.
You should add acid to amph free base to make a salt, not to p2np.
 

Montecristo

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awesome, thought something was up so i saved both phases i will sort out the solution later.
Do i have to completely evaporate off the ipa from the freebase or can i just bring it down to a workable level? ie 10%?
 

Montecristo

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what is the boiling point of amphetamine freebase?
 

Mclssmxxl

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awesome, thought something was up so i saved both phases i will sort out the solution later.
Do i have to completely evaporate off the ipa from the freebase or can i just bring it down to a workable level? ie 10%?
No need to evaporate at all if your organic layer is concentrated enough with product.If the freebase is too dilute it’s gonna precipitate like crap or not at all.I aim for 100ish ml organic layer first wash from 5g of propene.Then 1-2 more washes with 30-50 ml.
 

Mclssmxxl

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If you’re thinking of distilling I know for sure you need vaccum, maybe even inert atmosphere.It starts breaking down in the presence of air earlier than it’s boiling point as far as i can understand.Steam distill is what people go for commonly I think.
what is the boiling point of amphetamine freebase?
 

Montecristo

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okay thank you. and what would i do if there is too much solvent @ ph 6 and it doesnt precipitate? would it precipitate as it evaporates?
No need to evaporate at all if your organic layer is concentrated enough with product.If the freebase is too dilute it’s gonna precipitate like crap or not at all.I aim for 100ish ml organic layer first wash from 5g of propene.Then 1-2 more washes with 30-50 ml.
 

Mclssmxxl

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okay thank you. and what would i do if there is too much solvent @ ph 6 and it doesnt precipitate? would it precipitate as it evaporates?
I don’t know, I’ve only had it happen once, then I made sure i didnt have too big of a layer and that one time i didnt try to recouperate.Also phosphoric acid is trickier to get working than sulphuric.I recommend you find some of the latter.
 

Montecristo

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I don’t know, I’ve only had it happen once, then I made sure i didnt have too big of a layer and that one time i didnt try to recouperate.Also phosphoric acid is trickier to get working than sulphuric.I recommend you find some of the latter.
okay all good cheers. I have a battery sitting there too process, but i dont have time this run. i cannot buy sulphuric , but i can buy phosphoric ,so i have some. do you know what differences phosphoric may need?
 

ASheSChem

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how many % your phosphoric acid? if too much water with it, the yield decreases
 

Mclssmxxl

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okay all good cheers. I have a battery sitting there too process, but i dont have time this run. i cannot buy sulphuric , but i can buy phosphoric ,so i have some. do you know what differences phosphoric may need?
I heard from patton here that you should heat it up before.Something I’ve never done with sulphuric, but then again my acid is pretty pure.
Order from poland if you’re in the EU, they will sell you barrels of literally anything lol
 

Montecristo

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I heard from patton here that you should heat it up before.Something I’ve never done with sulphuric, but then again my acid is pretty pure.
Order from poland if you’re in the EU, they will sell you barrels of literally anything lol
okay thank you.
my country is risky compared to eu so id rather process a dead battery i have. which is fine, i just cbf at the moment and want to get this underway.
 

Montecristo

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if i add too much water, can i raise the ph back up to 11/12 to turn it back into freebase? and then separate & dry the solvent?
how many % your phosphoric acid? if too much water with it, the yield decreases
 

Montecristo

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should the ipa + freebase mix be cool when i acidify? should the acetone be chilled beforehand?
or does it not really mater if its going in the freezer for 12+ hours?
 
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