Synthèse de méthamphétamine à partir de P2P par réduction au NaBH4. Moyenne échelle.

[btcboss2022]

Bonjour,

Après de nombreux essais avec de la Méthylamine HCL basée sur cette méthode, je vais partager la meilleure façon que j'ai trouvée pour obtenir de la Méthamphétamine freebase à grande échelle :

• 966 gr P2P
• 14 litres de méthanol
• 1183 gr Méthylamine HCL
• 638 gr NaOH
• 452 gr Sulfate de sodium anhydre
• 105 gr NaBH4
• 35 L d'eau distillée
• 7 litres de DCM

- Remplir le réacteur avec les 14 litres de méthanol.
- Dissoudre la méthylamine HCL en agitant.
- Mettre la température du réacteur à 0C (pas la température du mélange) et ajouter le NaOH, la température va augmenter.
- Une fois que la température est revenue à 20°C, ajouter le P2P, la température augmentera. Remuer pendant 45min-1 heure.
- Ajouter 252gr de sulfate de sodium anhydre.
- Lorsque la température du mélange atteint 8°C, commencer à ajouter le NaBH4 par portions, sans dépasser 20°C.
- Une fois que tout le NaBH4 a été ajouté, laisser le mélange sous 20°C pendant environ 2 heures jusqu'à ce que le mélange cesse de faire des bulles.
- Ajouter l'eau et continuer à mélanger pendant 5 minutes
- Ajouter le DCM et mélanger pendant 10 minutes
- Arrêter de mélanger et laisser les couches se séparer
- Conserver la couche inférieure et jeter la couche supérieure (il n'est pas rentable d'extraire cette phase aqueuse)
- Ajouter 200gr de sulfate de sodium anhydre à la couche conservée et mélanger.
- Filtrer dans un entonnoir Buchner
- Evaporer le DCM
- Obtention d'une base libre de méthamphétamine propre et odorante

;-)

 

[snowbones]

Is the 35 litres of water added to ensure seperation of the dcm and water cos of the methanol present to stop it all mixing?
and are you using a 100 litre HDPE paint bucket as the reaction vessel?

 

[Chemistry lntern]

Excuse me! Is it necessary to use an ice bath when setting the reaction temperature to 0 degrees (not the temperature of the mixture

 

[Chemistry lntern]

Sir, may I ask if I know if the deep red liquid obtained after evaporating DCM is correct？

 

[Atompower]

Has any one trying this method of btc boss and had success with his write up

 

[William D.]

This looks like a working method, but some reagents and conditions can be changed.

 

[rage565]

Is there a video of this procedure available?

 

[G.Patton]

Have you tried to open Video section?

 

[Grubby]

Is 15g of NaBH4 enough as the reducing agent for 138g of P2P? Or should I add a small amount of reducing agent to avoid some side reactions?

 

[G.Patton]

Hello, yes it's not enough. You have to add at least equimolar amount 38.91g of NaBH4. It's even worth to add a little more, ~1.1 eqviv 42.8g.

 

[Grubby]

Idol, there must be a special reason why you choose to use less reducing agent! For example, to avoid certain side reactions or to favor certain steps? Please Master, please enlighten me on the mystery behind this.

 

[GnarleyBarley]

You don't need that much, 15 g (maybe a tiny bit more) is enough. 1 mol NaBH4 can reduce more than just 1 mol of imine. It can theoretically reduce 4 moles!!!

Don't know why patton says otherwise, but it's not true. and countless of articles, synthesis on forums and so on pretty much proves it

The following is for MDMA but the same molar ratio of NaBH4 applies to methamphetamine synthesis (here 0.47 equivalents is used)

 

[Chemistry lntern]

How does methylamine hydrochloride and methanol produce a 10% methylamine methanol solution

 

[GnarleyBarley]

Methylamine hydrochloride in methanol, add naoh.
You now need to filter the solution (NaCl is precipitated) and dry it with something (sieves, mgso4 etc). Filter it again
or just filter it one time after mgso4

Notice: More products are formed than what is shown in the table below (NaCl) is not shown because I don't care about how many grams of NaCl is produced, it will be filtered of anyway

CH6ClN = Methylamine hydrochloride, CH5N = methylamine, HNaO is NaOH (This table was made automatically in chemdraw, and this is how they do it.

As you can see, 26g of water is produced to make 45g methylamine from 98g of methylamine hydrochloride. Therefor you need something to dry up all the 26g of water (minimum)

I failed this reaction when I didn't dry it enough (because I didn't realize that so much water was actually produced (just added a little bit of mgso4 and thought I was good to go)

Also you don't need to have exactly 10% Methanol solution. Just enough to hold all the methylamine and enough to keep dilute the reaction enough.