Синтез метамфетамина из P2P путем восстановления NaBH4. Среднемасштабный.

[btcboss2022]

Здравствуйте,

После многих тестов с использованием Methylamine HCL, основанных на этом методе, я поделюсь лучшим способом, который я нашел для получения Methamphetamine freebase в больших масштабах:

• 966 гр P2P
• 14 литров метанола
• 1183 гр Метиламин HCL
• 638 гр NaOH
• 452 гр Безводный сульфат натрия
• 105 гр NaBH4
• 35 литров дистиллированной воды
• 7 литров DCM

- Заполните реактор 14 л метанола.
- При помешивании растворите метиламин HCL
- Поставьте температуру реактора на 0C (не температуру смеси) и добавьте NaOH, температура повысится.
- Как только температура вернется к 20C, добавьте P2P, температура увеличится, перемешивайте в течение 45 минут - 1 часа.
- Добавьте 252 грамма безводного сульфата натрия
- Когда температура смеси достигнет 8C, начните порционно добавлять NaBH4, не превышая 20C.
- После того, как весь NaBH4 будет добавлен, оставьте смесь перемешиваться при температуре 20C в течение примерно 2 часов, пока смесь не перестанет пузыриться
- Добавьте воду и продолжайте перемешивать в течение 5 минут
- Добавьте DCM и перемешивайте в течение 10 минут.
- Прекратите перемешивание и дайте слоям разделиться
- Сохраните нижний слой и выбросьте верхний (не выгодно извлекать эту водную фазу).
- Добавьте 200 г безводного сульфата натрия в сохраненный слой и перемешайте.
- Отфильтруйте на воронке Бюхнера
- Выпарите DCM
- Получено чистое и пахнущее свободное основание метамфетамина

;-)

 

[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.