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

Montecristo

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orthophosphoric acid yeilds amphetamine phosphate, which i what i was going for.
 

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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Please, don't spam!
 

G.Patton

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You should add acid to amph free base to make a salt, not to p2np.
 

Montecristo

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that is what i am talking about. is amp freebase+ipa on top layer after basifying?
 

ASheSChem

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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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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.
 

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?
 

Mclssmxxl

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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.
 

Montecristo

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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?
 

ASheSChem

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

Mclssmxxl

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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
 

Montecristo

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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?
 

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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