Synteza metamfetaminy z P2P poprzez redukcję NaBH4. Średnia skala.

[btcboss2022]

Witam,

Po wielu testach z użyciem metyloaminy HCL opartej na tej metodzie podzielę się najlepszym sposobem, jaki znalazłem, aby uzyskać wolną bazę metamfetaminy na dużą skalę:

• 966 gr P2P
• 14 litrów metanolu
• 1183 gr metyloaminy HCL
• 638 gr NaOH
• 452 gr Bezwodny siarczan sodu
• 105 gr NaBH4
• 35 l wody destylowanej
• 7 litrów DCM

- Napełnić reaktor 14 litrami metanolu.
- Mieszając rozpuścić metyloaminę HCL
- Ustaw temperaturę reaktora na 0C (nie temperaturę mieszaniny) i dodaj NaOH, temperatura wzrośnie.
- Gdy temperatura powróci do 20 ° C, dodaj P2P, temperatura wzrośnie, mieszaj przez 45 minut - 1 godzinę.
- Dodaj 252gr bezwodnego siarczanu sodu.
- Gdy temperatura mieszaniny osiągnie 8C, zacznij dodawać porcjami NaBH4, nie przekraczając 20C.
- Po dodaniu całego NaBH4 pozostaw mieszanie w temperaturze poniżej 20C przez około 2 godziny, aż mieszanina przestanie bulgotać.
- Dodać wodę i kontynuować mieszanie przez 5 minut
- Dodać DCM i mieszać przez 10 minut.
- Przestać mieszać i oddzielić warstwy
- Zachowaj dolną warstwę i odrzuć górną (nie opłaca się ekstrahować tej fazy wodnej).
- Dodaj 200 g bezwodnego siarczanu sodu do zachowanej warstwy i wymieszaj.
- Przefiltrować przez lejek Buchnera
- Odparować DCM
- Uzyskano czystą i śmierdzącą bazę wolną od metamfetaminy

;-)

 

[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？

 

[Chemistry lntern]

The taste is really good! Teacher, may I ask what the next step is for obtaining butter

 

[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.

 

[Chemistry lntern]

What is the next step to obtain butter？