Failed 4mmc synthesis

[Czeczeczecze]

I did 4mmc synthesis in DCM step by step like always. 1kg 2b4m 5L DCM 2L methyloamine, left it mixing for the night ~8h wash freebase 2 times, added ice 5L ice cold acetone with 500ml 35% hcl and nothing happened. Usually at the end of adding acetone with hcl powder is visible in whole solution. this time none. Any advice? whole batch is failed?

 

[ymaaah]

I see what u mean, the oil didnt precipitate thats right? If yes, just put the oil in a flat pyrex plate and wait some days, it will crystallize , after, u can purifiate it w/ acetone

 

[antrax]

I see what u mean, the oil didnt precipitate thats right? If yes, just put the oil in a flat pyrex plate and wait some days, it will crystallize , after, u can purifiate it w/ acetone

ymaaahDo you know if in the methylamination process of the organic base it is better to cover the beaker so that the methylamine fumes do not escape or leave the lid open so that the fumes escape?

 

[antrax]

I did 4mmc synthesis in DCM step by step like always. 1kg 2b4m 5L DCM 2L methyloamine, left it mixing for the night ~8h wash freebase 2 times, added ice 5L ice cold acetone with 500ml 35% hcl and nothing happened. Usually at the end of adding acetone with hcl powder is visible in whole solution. this time none. Any advice? whole batch is failed?

Czeczeczecze8 hours of stirring? I synthesize bk-MDMA and after the precursor CAS 52190-28-0 is dissolved with DCM and then I add the of methylamine 40% aqueous solution I stir it for 1 hour, then I do the extraction of ethyl acetate, I wash the free base 3 times and then add the 35-38% HCl & acetone solution to the free base and methylone HCl always comes out.

 

[xoxoxoxo]

8 hours of stirring? I synthesize bk-MDMA and after the precursor CAS 52190-28-0 is dissolved with DCM and then I add the of methylamine 40% aqueous solution I stir it for 1 hour, then I do the extraction of ethyl acetate, I wash the free base 3 times and then add the 35-38% HCl & acetone solution to the free base and methylone HCl always comes out.

antraxi made on dcm and i get 95g 4mmc powder form 100g 2b4m.
I was made your way and i get 30g only.....

 

[antrax]

i made on dcm and i get 95g 4mmc powder form 100g 2b4m.
I was made your way and i get 30g only.....

xoxoxoxoHow many accounts have you already created in this forum?

 

[rothschild33]

I did 4mmc synthesis in DCM step by step like always. 1kg 2b4m 5L DCM 2L methyloamine, left it mixing for the night ~8h wash freebase 2 times, added ice 5L ice cold acetone with 500ml 35% hcl and nothing happened. Usually at the end of adding acetone with hcl powder is visible in whole solution. this time none. Any advice? whole batch is failed?

CzeczeczeczeDid you add heating?

 

[xile]

@Czeczeczecze:
Same bro, never get a product of DCM-route.
Try Toluene or Benzen as a solvent and remember to use the upper layer. Acidify with a mixture of 90% Aceton and 10% HCL (37%).
A powder builds imediately amd you ust have to filter it.
Then recrystalate it.

 

[Jesse_Pinkman_]

@Czeczeczecze:
Same bro, never get a product of DCM-route.
Try Toluene or Benzen as a solvent and remember to use the upper layer. Acidify with a mixture of 90% Aceton and 10% HCL (37%).
A powder builds imediately amd you ust have to filter it.
Then recrystalate it.

xileBenzene is no good choice