Methamphetamin-Synthese aus P2P durch NaBH4-Reduktion. Mittelgroß.

[btcboss2022]

Hallo,

Nach vielen Versuchen mit Methylamin HCL, die auf dieser Methode basieren, werde ich den besten Weg teilen, den ich gefunden habe, um Methamphetamin freebase in großem Maßstab zu erhalten:

• 966 gr P2P
• 14 Liter Methanol
• 1183 gr Methylamin HCL
• 638 g NaOH
• 452 gr Wasserfreies Natriumsulfat
• 105 gr NaBH4
• 35 L destilliertes Wasser
• 7 Liter DCM

- Füllen Sie den Reaktor mit 14 l Methanol
- Lösen Sie das Methylamin HCL unter Rühren auf.
- Die Temperatur des Reaktors auf 0°C einstellen (nicht die Temperatur des Gemischs) und NaOH zugeben, die Temperatur wird ansteigen.
- Sobald die Temperatur wieder 20°C erreicht hat, fügen Sie das P2P hinzu, die Temperatur steigt und Sie rühren 45 Minuten bis 1 Stunde lang
- 252 g wasserfreies Natriumsulfat zugeben
- Wenn die Temperatur der Mischung 8°C erreicht hat, fügen Sie portionsweise NaBH4 hinzu, ohne die 20°C zu überschreiten.
- Sobald das gesamte NaBH4 zugegeben wurde, lässt man das Gemisch ca. 2 Stunden lang unter 20°C mischen, bis es nicht mehr blubbert.
- Fügen Sie das Wasser hinzu und mischen Sie 5 Minuten lang weiter
- DCM zugeben und 10 Minuten lang mischen
- Mit dem Rühren aufhören und die Schichten trennen lassen
- Die untere Schicht aufbewahren und die obere verwerfen (es lohnt sich nicht, diese wässrige Phase zu extrahieren)
- 200 g wasserfreies Natriumsulfat in die erhaltene Schicht geben und mischen
- In Buchner-Trichter filtrieren
- Das DCM verdampfen
- Saubere und stinkende Methamphetamin-Freebase erhalten

;-)

 

[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？