4mmc synthesis

[CristalKing]

DCM is also good but remember organic layer will be at the bottom and water layer will be UP:

1) Disolve 1 kg or 2-Br-3-chloropropiophenone or in 4 l DCM
2) Add to this 2 l of Methylamine 40% and mix it 4 h. If you are working with larger quantities for exaple 50 kg of 2br3 you have to give methylamine very slowly 1-1,5 h to keep the temperature no more then 39 degree ..., after add all methylamine mix it 3h
3) separate organic bottom layer and wash it 2 times by water.
4) Mix 0,390 ml HCl 37% with 300 ml of water
5) add solution of acid to organic layer and keep maximum about 20 degree. Mix it 15 min in large quantity longer ...(a precipitate of the final product may appear)
6)After 15 min heat everything to 39 degrees, until all the precipitate dissolves in the water layer. Stop stirring and keep the temperature at 39 degrees until the layers separate.
7) Decant the water layer and add 1200 ml of acetone to it. Bring everything to a gentle boil and then pour it into a crystallization cuvette. If nothing appears at room temperature, put the cuvette in the refrigerator at 5 degrees for 2 days.
We are waiting for a photos of final product...

 

[breathing.fire]

DCM is also good but remember organic layer will be at the bottom and water layer will be UP:

1) Disolve 1 kg or 2-Br-3-chloropropiophenone or in 4 l DCM
2) Add to this 2 l of Methylamine 40% and mix it 4 h. If you are working with larger quantities for exaple 50 kg of 2br3 you have to give methylamine very slowly 1-1,5 h to keep the temperature no more then 39 degree ..., after add all methylamine mix it 3h
3) separate organic bottom layer and wash it 2 times by water.
4) Mix 0,390 ml HCl 37% with 300 ml of water
5) add solution of acid to organic layer and keep maximum about 20 degree. Mix it 15 min in large quantity longer ...(a precipitate of the final product may appear)
6)After 15 min heat everything to 39 degrees, until all the precipitate dissolves in the water layer. Stop stirring and keep the temperature at 39 degrees until the layers separate.
7) Decant the water layer and add 1200 ml of acetone to it. Bring everything to a gentle boil and then pour it into a crystallization cuvette. If nothing appears at room temperature, put the cuvette in the refrigerator at 5 degrees for 2 days.
We are waiting for a photos of final product...

CristalKingWhy after put inside must cook without this You don't see two layers?

 

[WhalterWhite]

I added 300 ml of Hcl in 300 ml of freebase water quickly thickened with stirring and slow addition

 

[HairyPoppins]

I added 300 ml of Hcl in 300 ml of freebase water quickly thickened with stirring and slow addition

WhalterWhiteWhich method did you use? Dcm or toluene?

 

[little-flower]

Hello everybody"", I have test the reaction with toluen, but in the flask it is white, like milk when I put 2B4M in toluen,,,
is it good? is it a normal color?