Electrolytic reduction of P2NP to yield amphetamine

ItsMee

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I tried this methods before. It works, but yields are not so great but ok.
I got 2,5g - 3g sulphate from 5g P2NP
I used lead plates, cut from roofing lead. You have to use clean, blank surface on your electrodes.
Using porous clay pot for seperating your anode/cathode compartments works fine.
Anode compartment has to be filled with 12N sulfuric acid aswell.

Yes your mixture gets red. you have to remove it with non polar washings before basification.

What is important is temperature. in the paper it says not exceeding 40°C, but i experienced that this is too high.
Try to run it as cold as possible. Running your cell in an ice bath is an option. 10°C is prefered. and at the end you will see, that you just have a slightly red color. (less impurities, higher yield).

I tried this with max 10g P2NP, because my cell was that small. scaling up could be a problem because of heat generation.
You have to be creative in terms of active cooling than.

Trying this in a bucket with a big unglazed flowerpot would be awsome.

Maybe i will come up with a detailed procedure in future. unfortunately i cant provide pictures, because i tried this years before.

But hey, it is easy, non toxic and you need just common chemicals. But it takes time. you have to run your cell maybe for days, when you go large scale.
 

w2x3f5

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you can obtain sodium amalgam during the reaction (electroisynthesis), then the amalgam will remarkably restore your p2np
 

41Dxflatline

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I've been thinking, why do I need to cool the jar when I can just have constantly circulating anolyte in and out of my peltier coolers
 

ItsMee

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Circulating anolyte is a great option for cooling. Especially when you run the cell for long time.
Maybe the setup will be more complex but doable.
Hg Pool cathode should work fine, but i would prefer to avoid Hg in any cases. I think i will stay with lead electrode.

In the references it says always 0.2 A/cm².
Do you have an idea, if i should count both sides of the cathode, or just the side facing to the anode?
For example: A lead sheet with the measurements 2 cm x 5 cm.
Should this be counted as 10cm² or 20cm² ?
Because you have 10cm² on side of the cathode and 10cm² on the other side. This would make a huge difference.
 

41Dxflatline

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You count the surface area, so both sides. It doesn't matter that much anyway as long as it's close. 3amp would be fine for example. I'd just buy a reference electrode though if I were you, you don't need a potentiostat you can periodocially just adjust it by hand.
 

ItsMee

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I liked you cell design and now i am working on my own cell aswell. when i am done, i will show you, and maybe than you can explain me in detail, how to set this up with reference electrode and make the adjustments. electrochemistry is new for me. What kind of reference electrode is prefered in this setup? Ag/AgCl?
 
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