BENZILCIANİD (FENILACETONİTRİL) DO AMFETAMİNSULFAT

[ossi]

Pozdravljeni,

ali lahko strokovnjak morda napiše sintezno pot s snovmi, navedenimi spodaj?
primerna je za velik obseg in mislim, da je zanimiva za veliko ljudi tukaj

vsi reagenti so poceni in jih je lahko dobiti

• Benzilcianid (fenil acetonitril)
• žveplova kislina
• svinčev acetat trihidrat (ali druge alternative)
• formamid
• mravljinčna kislina
• HCİ
• natrijev hidroksid

Hvala vnaprej
ossi

 

[Hank Schrader]

Najlažji način za uporabo fenil acetonitrila je, da si priskrbite APAAN. Fenilacetonitril morate refluksirati v metanolu z natrijevim metilatom, po 6 urah refluksa morate pregnati ves metanol in vso oborino raztopiti v vodi ter med hlajenjem dodati ledeno ocetno kislino. Oborjeni APAAN večkrat speremo z vodo in rekristaliziramo v metanolu. Dobljeni beli kristal morate hidrolizirati v kislini (fosforjevi ali klorovodikovi), da dobite 860 ml P2P iz 1 litra fenilacetonitrila.

Za postopek pirolize, ki ga tako ali tako želite izvesti, je potrebna fenilocetna kislina, za njeno pridobitev pa morate tako ali tako hidrolizirati benzil cianid.
Ne bi se odločil za metodo, ki jo želite, in bi uporabil APAAN.
Čeprav v današnjem času obstajajo preprostejše metode kot APAAN in piroliza fenilocetnih soli ..

Kolikor vidim, želite uporabiti leukartovo reakcijo za izdelavo amfetamina.
Reakcija traja veliko časa in če želite narediti veliko proizvodnjo, potem pojdite po drugi poti.
Oglejte si nizkotlačno hidrogeniranje z uporabo kovinskih katalizatorjev.

Z Leukartovo reakcijo lahko proizvedete veliko izdelka, vendar reakcija zahteva razumevanje in veliko časa.
In praviloma proizvodnja začetnika dolgo časa ne bo presegla 50 % molske mase na keton.

 

[ossi]

zahvaljujem se vam za podroben odgovor.
Težava je v tem, da je to, kar se lahko naučite sami kot laik, omejeno.
v državi, kjer sem zdaj, se te snovi uporabljajo v množični proizvodnji. vendar me tukaj tega nihče ne uči.
Iščem leuckartovo metodo za velik obseg s snovmi, ki jih lahko dobite tudi vi. To metodo bi upravljal.
Materiale, ki sem jih omenil zgoraj, lahko zlahka dobim.
in 50 % je zame zelo dobro.

 

[yuiopjkl]

Našel sem to

 

[Jordan Belfort]

THF zamenjajte z nitrometanom in metanolom na 50/50 % aezotropa.


Vzemite primerno topilo, THF ali nitrometan (vendar morate preveriti, ali ne ustvarja metilamin), in dodajte magnezijeve ostružke ter pustite, da reagirajo z jodometanom, dokler se magnezijevi ostružki popolnoma ne raztopijo.
Tako boste dobili metilmagnezijev jodid.

Zdaj imate sintezo metamfetamina brez metilamina, vsa topila pa lahko destilirate in ponovno uporabite.

Če boste to naredili v enem loncu, kot pri Hg/Al Ga/Al, bo to verjetno preveč eksotermično in bo nastala zajebana zmeda. Predlagam, da na to počasi spustite keton.

Moram vam povedati, da to razmerje deluje za BMK z ultrazvokom.

 

[Jordan Belfort]

Oh, morda boste želeli povečati pH grignarda s čisto kavstično sodo na 8-9.

 

[caesare.robot]

Q zanima tudi, če ima kdo pozitiven odziv na to metodo ...

 

[yuiopjkl]

Nisem ga preizkusil.
Vprašajte strokovnjake. Morda imajo znanje in nasvete

@G.Patton @HIGGS BOSSON

 

[ossi]

in prosim, ali lahko nekdo skali za 1000gr?
@G.Patton @William Dampier @HEISENBERG

 

[G.Patton]

Za takšna vprašanja sem posebej napisal temo o molih, gramih, litrih in kemijskih izračunih
=> Kako šteti reagente?

 

[Hank Schrader]

To je neuporabna sinteza. Grignardov reagent, ogromne količine topil. To je, če je samo zaradi znanstvenega interesa, potem lahko to naredite 1 krat nič več. Za komercialno sintezo je brez vrednosti.

Z benzil cianidom je zelo enostavno dobiti fenilocetno kislino in v industrijskem obsegu narediti pirolizo soli, izkoristek ni največji, vendar je zelo priročen. Končni izdelek bo mešanica treh ketonov, ki jih je enostavno frakcionirati.

 

[Jordan Belfort]

Grignardovi reagenti so dejansko dobri. Še posebej, če dodate tudi cinkov klorid.

Če uporabljate ultrazvok, ne potrebujete brezvodnih reagentov.

 

[ossi]

bil bi vam neskončno hvaležen, če bi mi napisali sintezo s temi reagenti. vendar je za amaterja
40-50 % izkoristek v redu @Hank Schrader

 

[ossi]

Žal mi je, verjetno sem to spregledal, čeprav veliko berem tukaj

 

[FQ-BB]

List of reagents

- Use 12.65 kg of benzyl cyanide.
- Require 20 liters of concentrated sulfuric acid (H₂SO₄, 96%).
- Prepare 30 liters of deionized water.
- Use 18 liters of formamide.
- Require 12 liters of formic acid (HCOOH, 99%).
- Prepare 5 kg of sodium carbonate (Na₂CO₃).
- Use 5 liters of hydrochloric acid (HCl, 37%).
- Require 2 kg of sodium hydroxide (NaOH).
- Use 50 liters of dichloromethane (CH₂Cl₂).
- Optionally use 2 kg of lead acetate trihydrate (Pb(C₂H₃O₂)₂·3H₂O).

List of utensils and tools

- Use a 50-100 liter stainless steel or glass-lined reactor with a mechanical stirrer and equipped with temperature control (±2°C).
- Equip an industrial-grade condenser with a cooling circulation system.
- Equip an industrial-grade liquid separation device with a capacity of ≥10 liters.
- Install a large distillation tower with a condensing device and a collecting device with a capacity of ≥20 liters.
- Use an industrial Buchner funnel or filter press for solid-liquid separation.
- Prepare a corrosion-resistant storage tank with a capacity of ≥50 liters.
- Prepare a measuring cylinder (2 liters, 10 liters) and a beaker (500 ml to 5 liters).
- Use an industrial stirring device to ensure uniform mixing.
- Prepare a vacuum pump for vacuum distillation.
- Ensure that there are explosion-proof equipment, ventilation systems and fire extinguishers.
- Provide protective equipment such as protective gloves, goggles, gas masks and acid-proof aprons.

Step 1: Hydrolysis of benzyl cyanide to produce acetophenone

- Add 12.65 kg of benzyl cyanide and 30 liters of deionized water to the reactor, and start the agitator to make the solution uniform.
- Slowly add 20 liters of concentrated sulfuric acid in batches, and control the reaction temperature at 30-50°C to prevent violent exotherm.
- Heat the reaction mixture to 150°C for 1-2 hours and observe the color change from transparent to light brown.
- After cooling to room temperature, separate the acetophenone organic layer with a separatory funnel.
- Collect the 202°C fraction by distillation to obtain purified acetophenone.

Step 2: Acetophenone generates N-methylphenylethylamine through Leuckart reaction

- Add 13.05 kg of acetophenone and 18 liters of formamide to the reactor and start the agitator to mix evenly.
- Slowly add 12 liters of formic acid to ensure that the reactants are fully mixed.
- Heat to 120-140°C and maintain for 3-5 hours. The released gas is discharged through the condenser.
- After the reaction is completed, cool to room temperature and neutralize the mixture in a saturated solution of about 5 kg of sodium carbonate.
- Extract the reaction solution with 50 liters of dichloromethane in 5 times, dry and distill, collect the 194°C fraction, and obtain purified N-methylphenylethylamine.

Step 3: Post-treatment and purification

- Dissolve the purified N-methylphenylethylamine in a small amount of water and acidify to pH about 1 with 5 liters of hydrochloric acid to form the hydrochloride.
- If there are impurities, add 2 kg of lead acetate trihydrate, stir and filter the precipitate.
- Release the free N-methylphenylethylamine with 2 kg of sodium hydroxide solution, then extract it again with dichloromethane, dry and distill.

I reiterate that I am only a hobbyist and do not sell any precursors or substances. Anyone violating escrow transactions is a scammer.

Respect to BB administrators. Salute 🫡

 

[G.Patton]

Napisal sem ga pred nekaj dnevi.

 

[FQ-BB]

Is there a reward?

 

[FQ-BB]

I'll challenge

 

[FQ-BB]

List of reagents

- Use 12.65 kg of benzyl cyanide.
- Require 20 liters of concentrated sulfuric acid (H₂SO₄, 96%).
- Prepare 30 liters of deionized water.
- Use 18 liters of formamide.
- Require 12 liters of formic acid (HCOOH, 99%).
- Prepare 5 kg of sodium carbonate (Na₂CO₃).
- Use 5 liters of hydrochloric acid (HCl, 37%).
- Require 2 kg of sodium hydroxide (NaOH).
- Use 50 liters of dichloromethane (CH₂Cl₂).
- Optionally use 2 kg of lead acetate trihydrate (Pb(C₂H₃O₂)₂·3H₂O).

List of utensils and tools

- Use a 50-100 liter stainless steel or glass-lined reactor with a mechanical stirrer and equipped with temperature control (±2°C).
- Equip an industrial-grade condenser with a cooling circulation system.
- Equip an industrial-grade liquid separation device with a capacity of ≥10 liters.
- Install a large distillation tower with a condensing device and a collecting device with a capacity of ≥20 liters.
- Use an industrial Buchner funnel or filter press for solid-liquid separation.
- Prepare a corrosion-resistant storage tank with a capacity of ≥50 liters.
- Prepare a measuring cylinder (2 liters, 10 liters) and a beaker (500 ml to 5 liters).
- Use an industrial stirring device to ensure uniform mixing.
- Prepare a vacuum pump for vacuum distillation.
- Ensure that there are explosion-proof equipment, ventilation systems and fire extinguishers.
- Provide protective equipment such as protective gloves, goggles, gas masks and acid-proof aprons.

Step 1: Hydrolysis of benzyl cyanide to produce acetophenone

- Add 12.65 kg of benzyl cyanide and 30 liters of deionized water to the reactor, and start the agitator to make the solution uniform.
- Slowly add 20 liters of concentrated sulfuric acid in batches, and control the reaction temperature at 30-50°C to prevent violent exotherm.
- Heat the reaction mixture to 150°C for 1-2 hours and observe the color change from transparent to light brown.
- After cooling to room temperature, separate the acetophenone organic layer with a separatory funnel.
- Collect the 202°C fraction by distillation to obtain purified acetophenone.

Step 2: Acetophenone generates N-methylphenylethylamine through Leuckart reaction

- Add 13.05 kg of acetophenone and 18 liters of formamide to the reactor and start the agitator to mix evenly.
- Slowly add 12 liters of formic acid to ensure that the reactants are fully mixed.
- Heat to 120-140°C and maintain for 3-5 hours. The released gas is discharged through the condenser.
- After the reaction is completed, cool to room temperature and neutralize the mixture in a saturated solution of about 5 kg of sodium carbonate.
- Extract the reaction solution with 50 liters of dichloromethane in 5 times, dry and distill, collect the 194°C fraction, and obtain purified N-methylphenylethylamine.

Step 3: Post-treatment and purification

- Dissolve the purified N-methylphenylethylamine in a small amount of water and acidify to pH about 1 with 5 liters of hydrochloric acid to form the hydrochloride.
- If there are impurities, add 2 kg of lead acetate trihydrate, stir and filter the precipitate.
- Release the free N-methylphenylethylamine with 2 kg of sodium hydroxide solution, then extract it again with dichloromethane, dry and distill.

I reiterate that I am only a hobbyist and do not sell any precursors or substances. Anyone violating escrow transactions is a scammer.

Respect to BB administrators. Salute 🫡

 

[tin ton]

* Benzylacetone → Hydrazine (NH₂NH₂) Condensation → Strong Alkali Reduction → P2P

Steps:
Benzylacetone (10 g) anhydrous hydrazine (NH₂NH₂·H₂O, 98%) 15 m potassium hydroxide (KOH) 10 g ethylene glycol (solvent) 50 mL
- In a flask, add benzylacetone and anhydrous hydrazine, reflux and stir for 3 hours.Add KOH, heat up to 180°C and continue heating for 2 hours (Wolff-Kishner reduction). Cool down, extract, and distill (202-205°C) to collect P2P.Key point: Wolff-Kishner requires high temperature (180°C), avoid rapid heating.

 

[FQ-BB]

* Benzylacetone → Hydrazine (NH₂NH₂) Condensation → Strong Alkali Reduction → P2P

Steps:
Benzylacetone (10 g) anhydrous hydrazine (NH₂NH₂·H₂O, 98%) 15 m potassium hydroxide (KOH) 10 g ethylene glycol (solvent) 50 mL
- In a flask, add benzylacetone and anhydrous hydrazine, reflux and stir for 3 hours.Add KOH, heat up to 180°C and continue heating for 2 hours (Wolff-Kishner reduction). Cool down, extract, and distill (202-205°C) to collect P2P.Key point: Wolff-Kishner requires high temperature (180°C), avoid rapid heating.