Metamfetamiinisynteesi P2P:stä NaBH4-pelkistyksellä. Keskisuuri mittakaava.

[btcboss2022]

Hei,

Monien metyyliamiini HCL: ää käyttävien testien jälkeen, jotka perustuvat tähän menetelmään, jaan parhaan tavan, jonka löysin metamfetamiinin vapaan pohjan saamiseksi suuressa mittakaavassa:

• P2P
• 14 litraa metanolia
• 1183 gr metyyliamiini HCL
• 638 gr NaOH
• 452 gr Vedetön natriumsulfaatti
• 105 gr NaBH4
• 35 l tislattua vettä
• 7 litraa DCM

- Täytetään reaktori 14 litralla metanolia.
- Liuotetaan sekoittaen metyyliamiini HCL:ää
- Laita reaktorin lämpötila 0 C:een (ei seoksen lämpötila) ja lisää NaOH, lämpötila nousee.
- Kun lämpötila on noussut takaisin 20 C:een, lisätään P2P, lämpötila nousee ja sekoitetaan 45 minuutin-1 tunnin ajan.
- Lisätään 252 g vedetöntä natriumsulfaattia.
- Kun seoksen lämpötila nousee 8 C:een, aletaan lisätä NaBH4:ää annoksittain, mutta ei yli 20 C:n.
- Kun kaikki NaBH4 on lisätty, annetaan seoksen sekoittua 20 C:ssa noin 2 tunnin ajan, kunnes seos lakkaa kuplimasta.
- Lisätään vesi ja jatketaan sekoittamista 5 minuutin ajan.
- Lisätään DCM ja sekoitetaan 10 minuutin ajan.
- Lopetetaan sekoittaminen ja annetaan kerrosten erottua toisistaan
- Pidetään alempi kerros ja hylätään ylempi (tätä vesifaasia ei kannata uuttaa).
- Lisätään 200 grammaa vedetöntä natriumsulfaattia säilytettyyn kerrokseen ja sekoitetaan.
- Suodatetaan Buchnerin suppiloon
- Haihdutetaan DCM
- Saadaan puhdas ja haiseva metamfetamiinivapaa emäs.

;-)

 

[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？