4mmc synthesis

[WhalterWhite]

We need:
-1 kg 2bromo 4 metylopropiofenon
- 4 l toulen
- 3.5 l metyloamina
- aceton


1.Add to the reactor 2B4M.Next add pour toulen and wait until the Dissolves.

2.Add slowly methylamine and stir heating 90 minutes in 40°, after this time off heating and still mix 30 min.

3. Stop stirring, waiting for the mixture to split into two layers.the top layer remains. Rinse with water 1-2 times.

4.Add mix wather 2 l and hydrochloric acid 750 ml and add to the mixture.

Now different methods were tested:
1. method. Pour the mixture into plates and dry with air. When it is dry clean with acetone and we get the powder. By this method, 74% of the powder yield was obtained in a small amount.

2. Method
We add to mixture caustic soda 340 g with water 800 ml coold. And when separate
Now the pure mephedrone will separate from the water. Mephedrone goes up. Separate mephedrone and add 2l of methanol + 400 ml of hydrochloric acid to it.We should have about 750 ml of pure mephedrone in solution. We pour it on plates and wait for it to dry. Then we spit with acetone and we have the powder.

3. Method.

The third method is with cold acetone and hydrochloric acid, but I did not try and I do not know the proportions

 

[WhalterWhite]

But when use 40° all going good. Is more better in 60° ?

 

[Uncle Lee]

You'd better use DCM as the solvent for the reaction, if you use benzene and the reaction temperature is high or the reaction time is too long, it will produce harmful impurities such as pyrazine

 

[CristalKing]

yeld 74% was good, but in final product you have a lot of methylamine HCL. Final product with a lot of methylamine HCl is difficult to recrystalization and to get nice big needles, only small cristalline powder. To the reaction you use to much methylamine, should be max x2 to 2Br4 so 2 l, and to much HCL, schould be maximum 415 ml for 1 kg of 2br4 optimal is 0,38 ml HCl of 37%. If you will give more acid final product will be more white but ph will be lower 1-2.

 

[WhalterWhite]

You'd better use DCM as the solvent for the reaction, if you use benzene and the reaction temperature is high or the reaction time is too long, it will produce harmful impurities such as pyrazine

Uncle LeeI just have a dcm barrel. I don't know how to do it. What time, what temperature? Can you help me? Now i trying make 2b3chloro liquid. Regards

 

[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]

Thank You. Give me 1 week

 

[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...

CristalKingSorry, I made little mistake. Please add 400-415 g of 37% HCL acid for 1 kg of Br, not 390 ml becouse it is a little to much. ( g not ml ) ! If you are doing small amount you can give 400g if amout is bigger use better 410-415 g HCL for 1 kg br becouse reaction is a little exotermic and a little hcl gas can go to air ......

 

[WhalterWhite]

How much in ml, 400g of hydrochloric acid?

 

[Pan Cyga]

Can methylamine solution be 30%? I can access only that.

 

[CristalKing]

How much in ml, 400g of hydrochloric acid?

WhalterWhiteDensity of 37% HCL is about 1,19g/ml, So 400/1,19=336 ml

 

[johnny.b]

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...

CristalKingIs better to mix HCl with water and separate layers or HCl 33-35% without water and without mix with acetone will be work to?

 

[Chenzen]

Use aceton and hcl is better like you use water

 

[johnny.b]

Use aceton and hcl is better like you use water

ChenzenCan You tell me what proportions will be good to mix HCL and acetone.
I see people use 1:8 event 1 :10 less will be not work?

 

[johnny.b]

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...

CristalKingThis down layer for sure You can throw away there is nothing good staff?

 

[johnny.b]

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...

CristalKingI do everything like in Your recipe and this is still liquid aby idea?

 

[Netflix]

2 times washing water alone is not enough rinsing should be from 3 to 5 water must not be empty at the end and why water and hydrochloric acid then need a lot of smearing too much work and smells

 

[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?

 

[WhalterWhite]

What can be done now, how to fix it?

 

[Didi]

With Aceton wash simple