BENZILCIĀNİD (FENILACETONİTRİL) LĪDZ AMFETAMĪNȦNSULFĀTAM

[ossi]

Sveiki,

vai kāds eksperts, iespējams, var uzrakstīt sintēzes maršrutu ar turpmāk uzskaitītajām vielām?
tas ir labi piemērots lielam mērogam, un es domāju, ka tas ir interesants daudziem cilvēkiem šeit

visi reaģenti ir lēti un viegli iegūstami

• Benzilcianīds (fenilacetonitrils)
• sērskābe
• svina acetāta trihidrāts (vai citas alternatīvas)
• formamīds
• skudrskābe
• HCİ
• nātrija hidroksīds

iepriekš paldies
ossi

 

[Hank Schrader]

Visvienkāršākais veids, kā jūs varat lietot fenilacetonitrilu, ir iegūt APAAN. Fenilacetonitrils jums ir jārefluksē metanolā ar nātrija metilātu, pēc 6 stundu refluksa jānodzen viss metanols un visas nogulsnes jāizšķīdina ūdenī, un atdzesējot jāpievieno ledus etiķskābe. Izgulsnēto APAAN vairākas reizes mazgā ar ūdeni un pārkristalizē metanolā. Iegūto balto kristālu hidrolizē skābē (fosforskābē vai sālsskābē), lai no 1 litra fenilacetonitrila iegūtu 860 ml P2P.

Pirolīzes procesam, ko jūs jebkurā gadījumā vēlaties veikt, ir vajadzīga fenilacetskābe, un, lai to iegūtu, jums tik un tā ir jāhidrolizē benzilciānīds.
Es neizvēlētos jūsu izvēlēto metodi un izmantoju APAAN.
Lai gan mūsdienās ir vienkāršākas metodes nekā APAAN un feniletiķskābes sāļu pirolīze ..

Cik es saprotu, jūs vēlaties izmantot leikarta reakciju, lai iegūtu amfetamīnu.
Reakcija aizņem daudz laika, un, ja vēlaties veikt lielu ražošanu, tad ejiet citu ceļu.
Skatīt zemspiediena hidrogenēšanu, izmantojot metāla katalizatorus.

Ar Leukarta metodi var iegūt daudz produktu, bet reakcija prasa izpratni un daudz laika.
Un parasti iesācēja produkcija ilgu laiku nepārsniegs 50 % pēc molmasas uz ketonu.

 

[ossi]

Paldies par detalizētu atbildi.
Problēma ir tā, ka tas, ko jūs kā nespeciālists varat iemācīties pats, ir ierobežots.
Valstī, kurā es pašlaik atrodos, šīs vielas tiek izmantotas masveida ražošanā. bet šeit neviens man to nemāca.
Es meklēju leikarta metodi lieliem mērogiem ar materiāliem, ko var arī dabūt. Es pārvaldītu šo metodi.
Es varu viegli iegūt iepriekš minētos materiālus.
un 50% man ir ļoti labi.

 

[yuiopjkl]

Es atradu šo

 

[Jordan Belfort]

Aizstājiet THF ar nitrometānu un metanolu 50/50% aezotropā.


Vai nu ņem piemērotu šķīdinātāju, THF, vai nitrometānu (bet jāpārbauda, vai tas nav grūti radošs metilamīns), pievieno magnija skaidas un ļauj tām reaģēt ar jodmetānu, līdz magnija skaidas pilnībā izšķīst.
Tas jādara tikai, lai iegūtu metilmagnija jodīdu.

Tagad jums ir 1 katls metamfetamīna sintēzes bez metilamīna, un jūs varat destilēt visus šķīdinātājus un izmantot atkārtoti.

Veicot to vienā katlā, piemēram, ar Hg/Al Ga/Al, iespējams, būs pārāk liels eksotermiskums un radīsies draņķīgs haoss. Es iesaku lēnām pilienu ketonu uz to.

Man jums jāsaka, ka šī attiecība darbojas BMK ar ultraskaņu.

 

[Jordan Belfort]

Ak, iespējams, jūs vēlaties palielināt grignarda pH ar tīru kaustisko sodu līdz 8-9.

 

[caesare.robot]

Q arī interesē, ja kādam ir pozitīva atbilde par šo metodi ...

 

[yuiopjkl]

Es neesmu to izmēģinājis.
Jautājiet ekspertiem. Viņiem var būt zināšanas un padomi

@G.Patton @HIGGS BOSSON

 

[ossi]

un, lūdzu, vai kāds var mērogot 1000gr?
@G.Patton @William Dampier @HEISENBERG

 

[G.Patton]

Šādiem jautājumiem es uzrakstīju īpašu tēmu Moles, grams, litri un ķīmiskie aprēķini.
=> Kā aprēķināt reaģentus?

 

[Hank Schrader]

Šī ir nelietderīga sintēze. Grignarda reaģents, milzīgs daudzums šķīdinātāju. Tas ir, ja tikai zinātniskas intereses dēļ, tad to var darīt 1 reizi ne vairāk. Komerciālai sintēzei nav nekādas vērtības.

Ja ir benzilciānīds, ir ļoti viegli iegūt fenilpienskābi, un rūpnieciskā mērogā veikt sāļu pirolīzi, iznākums nav vislielākais, bet ļoti ērts. Galaproduktā būs triju ketonu maisījums, ko ir viegli frakcionēt.

 

[Jordan Belfort]

Grignarda reaģenti patiešām ir labi. Īpaši, ja pievieno arī cinka hlorīdu.

Ja izmantojat ultraskaņu, jums nav vajadzīgi bezūdens reaģenti.

 

[ossi]

es būtu bezgala pateicīgs, ja jūs man uzrakstītu sintēzi ar šiem reaģentiem. bet amatierim
40%-50% iznākums ir ok @Hank Schrader

 

[ossi]

Atvainojiet, es droši vien to esmu palaidis garām, lai gan daudz lasīju šeit

 

[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]

Es to uzrakstīju pirms pāris dienām.

 

[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.