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

[Pajmon]

Lately, I have not been able to get this reaction. I don't know what I'm doing wrong. Before that, I had better results. I always make only a lot of 10 grams, I don't know what I'm doing wrong, maybe someone can help. I have the ratio of substances as in the video, I use a half-liter flask with 3 holes - thermometer, cooler and hole where I put it. I use magnetic stirring. I think that's enough for that amount. In the first phase, my temperature is around 40-50 degrees, every time it starts to drop, I make a match. I tried 2 but also 4 hours with the same result. In the second phase, when I add a small amount, my temperature does not rise, as a result I have maybe half a gram. Before that, I used to have 5-6 grams. After adding H3PO4 drops, the whole thing thickened, now only a little bit is formed. I don't know what I'm doing wrong

 

[G.Patton]

Hi. Did you ad CuCl2 and reach this temperature?

 

[Pajmon]

The color of CuCl2 is the same as in the video, and I only added a few drops of acid, but there was a lot of ice. I don't know what I'm doing wrong, everything looks good, the temperature has also risen after adding CuCl2, you need to have a higher temperature than I had. A-oil looks good, but I can't get amphetamine... and I'm gradually lowering the pH to 5.

 

[G.Patton]

As I see, the problem with acidification procedure. You should reach pH6, not less.

So, you get a-oil, separate it from IPA and did everything like in the method?

 

[mile123]

Hello @GhostChemist

I have 5g p2np batch,
I'm at step 8,

8. The IPA from step 7 extract is evaporated on vacuum to an amphetamine free base oil and combined with free base from step 6.

I add 80ml of ipa to wash it.
I locked vacuum at 600mmHg, 800 millibars, I have gauge on vacuum pump inlet.
My distillation setup is 3 necked flask, vertical alihn reflux condesner as fraction column, horizontal grahm condeser as cooling. I can confirm by flame I get IPA.

I get liquid with milky aqueous layer and yellow top which isn't possible to lower PH with H2SO4. I think I over distill it.
1. IPA evaporates at 69°, it goes for 8h and doesn't stop, what may be indicator when it is done?

2. What would happen if I don't wash aqueous layer with IPA and just proceed with dropwise addition of H2SO4?

 

[GhostChemist]

General procedure for this synthesis is separate IPA with amine and distilled off the IPA for concentation of amine

 

[darknessss]

@
@GhostChemist can I replace the IPA with denatured EtOH so i have a freebase solution with EtOH at the end so I can make Amphetamine sulfate paste because everyone wants paste nowadays!

 

[GhostChemist]

You can not use EtOH instead IPA in stage 1-8

 

[darknessss]

Thanks for the reply

 

[Pajmon]

It's not urine

 

[mile123]

Is it aqeous layer at bottom, will you evaporate IPA or continue without washing?

 

[GhostChemist]

Interesting