Синтез на метамфетамин от P2P чрез редукция с NaBH4. Среден мащаб.

[btcboss2022]

Здравейте,

След много тестове с използване на Methylamine HCL въз основа на този метод ще споделя най-добрия начин, който открих за получаване на Methamphetamine freebase в голям мащаб:

• 966 gr P2P
• 14 литра метанол
• 1183 gr Methylamine HCL
• 638 gr NaOH
• 452 gr Безводен натриев сулфат
• 105 gr NaBH4
• 35 л дестилирана вода
• 7 литра DCM

- Напълнете реактора с 14 л метанол
- При разбъркване се разтваря Methylamine HCL
- Поставете температурата на реактора на 0С (не температурата на сместа) и добавете NaOH, температурата ще се увеличи
- След като температурата се върне на 20С, добавете P2P, температурата ще се повиши, разбърквайте в продължение на 45 минути - 1 час
- Добавете 252 g безводен натриев сулфат
- Когато температурата на сместа достигне 8С, започнете да добавяте на порции NaBH4, като не превишавате 20С
- След като добавите всички количества NaBH4, оставете сместа да се разбърква при температура под 20С в продължение на около 2 часа, докато сместа спре да бълбука
- Добавете водата и продължете да разбърквате в продължение на 5 мин.
- Добавя се DCM и се разбърква в продължение на 10 мин.
- Преустановете разбъркването и оставете слоевете да се отделят
- Запазете долния слой и изхвърлете горния (не е изгодно да се извлича тази водна фаза)
- Добавете 200 g безводен натриев сулфат към запазения слой и го разбъркайте
- Филтрирайте с фуния на Бюхнер
- Изпарявайте DCM
- Получава се чиста и миризлива свободна метамфетаминова база

;-)

 

[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.