p2np nabh4 amfetamiini sünteesi küsimus

[SoldadoDeDrogas]

Tuco mu sõber,
Ma vaatasin ühe poti sünteesi retsepti ja CuCl2/H2O lahuse suhe on 1/2, mis tähendab, et 200mg CuCl2 jaoks kasutaksite 400mg H2O lahuse proportsioonina.
Temperatuur ei tõuse ehk sellepärast, et see on nii väike skaala. Samuti kasutate te kaheliitrist kolbi - suht suur selleks, millega te töötate, mitte?
Pärast CuCl2 lahuse lisamist hoitakse temperatuur 30 minutit välise kuumutamise abil 80c juures. Kas sul on kuumutusplaat, mida saad valida?
Lisa oma NaOH lahus alusele. Eralda vesifaas IPA abil ja redutseeri vaakumiga tagasi vababaasiks.
Lahustage vababaas atsetoonis ja lisage H2SO4, kuni pH on 6.
Asetage sügavkülma ~12 tunniks
Koguge sool kokku ja peske külma kuiva atsetooniga, kuni see on valget värvi.

Kui teil on ikka veel probleeme nende portsjonitega, soovitan kasutada suuremat partiid. See on 45-leheküljeline teema ja see ei ole ainus. Seal peab olema rohkem infot, mida saate kasutada. Loe, vend.

 

[TucoSalamanca.]

Ütlen teile, kuidas seda teha, kõigepealt lisan 10ml ipa 80ml h2o, siis lisan 3,5gr nabh4, siis lisan 2gr p2np, mitte üle 60 kraadi, siis lahustan vaskkloriidi 456mg 1ml vees ja lisan seda, mitte üle 80 kraadi, siis kuumutan seda 80 kraadi 30 minutit, võtan ülemise kihi ja lisan lahuse 16ml veega 25% naoh, siis teen ph 6 ja panen selle sügavkülma.

 

[SoldadoDeDrogas]

Pärast freebaseerimist NaOH lahusega. Lisate IPA-d, et lahustada freebase veekihi sisse. Eraldage veekiht ja aurustage, et saada freebase tagasi.
Seejärel lisage freebase atsetoonile ja lisage H2SO4 kuni pH 6 - Seejärel võite asetada sügavkülma. Tekivad tahked ained ja te filtreerite. Peske tahked ained külma kuiva atsetooniga kuni valge värvuseni.

 

[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.