p2np nabh4 amphetamine synthesis question

[SoldadoDeDrogas]

Tuco my friend,
I looked at the one pot synth recipe and the CuCl2/H2O solution is in 1/2 ratio meaning for 200mg CuCl2 you would use 400mg H2O as your solution proportion.
The temperature does not increase perhaps because it is such a small scale. Also you are using a two liter flask - kind of big for what you are working with, no?
After the CuCl2 solution is added, the temperature is maintained at 80c for 30 minutes with help of external heating. You got a hot plate you can dial in?
Add your NaOH solution to base. Seperate aqueous phase using IPA and reduce back into freebase with a vacuum.
Dissolve freebase into acetone and add H2SO4 until pH 6.
Place in freezer for ~12 hours
Collect salt and wash with cold dry acetone until it is white colored.

If you are still having trouble with these portions I would suggest using a larger batch. That is a 45 page thread, and it is not the only one. There has to be more info in there you can use. Read, brother.

 

[TucoSalamanca.]

Let me tell you how to do it, first I will add 10ml ipa 80ml h2o, then I will add 3.5gr nabh4, then I will add 2gr p2np, not exceeding 60 degrees, then I will dissolve copper chloride 456mg in 1ml water and add it, not exceeding 80 degrees, then I will heat it to 80 degrees for 30 minutes, I will take the top layer and add the solution with 16ml water 25% naoh, then I will make ph 6 and put it in the freezer.

 

[SoldadoDeDrogas]

After freebasing with NaOH solution. You will add IPA to dissolve the freebase into the water layer. Seperate the water layer and evaporate to get the freebase back.
Then add freebase to acetone and add H2SO4 until pH 6 - Then you may place into freezer. Solids will form and you will filter. Wash solids with cold dry acetone until white color.

 

[Chemdogkm]

Smalllllll scale. Had good success with nabh4 synth at p2np 10g scale,but yield was only 20%

 

[GhostChemist]

yield in AMP synthesis (P2NP+NaBH4) must be 60-70%
http://bbzzzsvqcrqtki6umym6itiixfhn...esis-from-p2np-with-nabh4-cucl2-1kg-scale.70/

 

[OneTensionSkyRed]

I have some interesting information on NaBH4/Cu reduction of nitropropenes. Some say that this reaction produces hydroxylamine as the main product or even as the only product. The reason is that nitropropenes are harder to reduce unlike nitrostyrenes. So NaBH4/Cu gives phenylethylamine when reducing phenyl-2-nitrostyrene but with p2np it gives N-OH instead of amine - or at least a large part of the product is N-OH with some part as amine. The problem is that amphetamine and it's hydroxylamine have very similar boiling points and melting points for their salts and they're hard to separate and analyse.
People are saying that p2np reduced by amalgam and the same p2np reduced by NaBH4/Cu have very distinct effects for users.
Can anyone confirm or debunk this? Has anyone tried analysing the product by TLC?

 

[waltjr5858]

Agreed but only the way most people run it... it will make full ampehtamine but the size and shape of the catalyst is extremely important for it to really work. Otherwise stuck with that intermediate. If the copper is just dumped into an unknown quantity of nabh4 in solution yes hydroxylamine will most likely be the product....call it almost ampehtamine. Best way is to use thf and methanol 10:1 and get the 1-phenyl-2-nitropropane intermediate with no addition reaction this way. Then destroy remaining nabh4 and isolate propane. Dissolve in the normal 2:1 isopropanol water and now we will be using a set amount of nabh4 to make proper cu nanoparticles which will absolutely reduce fully. A little finely ground carbon will also raise catalyst activity greatly. Use ratio of 1:2:0.15 for each mole of propane use 2 moles of nabh4 and 0.15 copper with about the same activated carbon. So little bits and your catalyst should start as brownish color. With the catalyst it is just increasing surface area and absorbing hydrogen and the meditates an electron transfer.... 30 mins 80c... boom fully reduced. I would practice on solvent volume to get that brown to brown red catalyst color. Without complicated equipment that's the only way I can tell the catalyst will function the way i want. I have it written down somewhere how much alcohol and water to use per gram of nabh4... that's what really matters. Don't want the copper reduced all the way immediately and inactive. I'll look.