BENZYLCYANİD (PHENYLACETONİTRİL) TO AMPHETAMİNSULFAT

[ossi]

hello,

can an expert perhaps write a synthesis route with the substances listed below?
it's well suited for big scale, and I think it's interesting for a lot of people here

all reagents are cheap and easy to get

• Benzylcyanid (Phenylacetonitril)
• sulfuruc acid
• lead acetate trihydrate (or other alternatives)
• formamide
• formic acid
• HCİ
• Sodium hydroxide

thanks in advance
ossi

 

[Hank Schrader]

The easiest way for you to use phenylacetonitrile is to get APAAN. Phenylacetonitrile you need to reflux in methanol with sodium methylate, after 6 hours of reflux you need to drive off all the methanol and dissolve all the precipitate in water, and add glacial acetic acid while cooling. The precipitated APAAN was washed several times with water and recrystallized in methanol. The resulting white crystal you need to hydrolyze in acid (phosphoric or hydrochloric) get 860 ml P2P from 1 liter of phenylacetonitrile.

The pyrolysis process that you want to do anyway requires phenylacetic acid, and to get it you need to hydrolyze benzyl cyanide anyway.
I would not go with the method you want and would use APAAN.
Although in our time there are simpler methods than APAAN and pyrrolysis of phenylacetic salts ..

As far as I can see, you want to use the leukart reaction to make amphetamine.
The reaction takes a lot of time and if you want to do a large production, then go the other way.
See low pressure hydrogenation using metal catalysts.

A lot of product can be produced with Leukart, but the reaction requires understanding and a lot of time.
And as a rule, the output of a beginner will not exceed 50% by molar mass per ketone for a long time.

 

[ossi]

thank you for the detailed answer.
The problem is that what you can teach yourself as a layman is limited.
in the country where i am right now, these substances are used in mass production. but nobody teaches me that here.
i'm looking for a leuckart method for a large scale with materials that you can also get. I would manage this method.
I can easily get the materials I mentioned above.
and 50% is very good for me.

 

[yuiopjkl]

I found this

 

[Jordan Belfort]

Replace THF with nitromethane and methanol on 50/50% aezotrope.


Either you take an suitable solvent, THF, or nitromethane(but you have to check if it's isn't hardcore generating methylamine), and add magnesium shavings and let them react with iodomethane till magnesium shavings fully dissolve.
This is only to make your methylmagnesium iodide.

Now you have 1 pot synthese to methamphetamine without methylamine and you can distill all solvents and reuse.

Doing this onepot like with Hg/Al Ga/Al will probably be to exothermic and make a fucking mess. I suggest you drop slowly the ketone on it.

I must tell you this ratio works for BMK with ultrasound.

 

[Jordan Belfort]

Oh you may want to increase the pH of the grignard with pure caustic soda to 8-9.

 

[caesare.robot]

Q is also interested if someone has positive response on this method ...

 

[yuiopjkl]

I haven't tried it.
Ask the experts. They may have knowledge and advice

@G.Patton @HIGGS BOSSON

 

[ossi]

and please can someone scale for 1000gr?
@G.Patton @William Dampier @HEISENBERG

 

[G.Patton]

I wrote Moles, grams, litres and chemical calculations topic special for such questions
=> How to count reagents?

 

[Hank Schrader]

This is a useless synthesis. Grignard reagent, huge amounts of solvents. This is if only for scientific interest, then you can do it 1 time no more. For commercial synthesis is of no value.

Having benzyl cyanide, it is very easy to obtain phenylacetic acid, and on an industrial scale to do pyrrolysis of salts, the yield is not the highest, but very convenient. The final product will have a mixture of three ketones that are easy to fractionate.

 

[Jordan Belfort]

Grignard reagents actually are good. Especially if you add zinc chloride also.

If you use ultrasound you don't need anhydrous reagents.

 

[ossi]

i would be infinitely grateful if you would write me a synthesis with these reagents. but for an amateur
40%-50% yield is ok @Hank Schrader

 

[ossi]

sorry, I must have overlooked it, although I read a lot here

 

[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]

I wrote it couple day ago.

 

[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.