WillD
Expert
- Joined
- Jul 19, 2021
- Messages
- 645
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- 93
How many methylamine did u end up using in the cmc-synth?
You can use a similar quantities
How many methylamine did u end up using in the cmc-synth?
You can use a similar quantities
We already did a succesfull synthesis of 3cmc. The help was greatly appreciated.
Reaction scheme:
View attachment 1218
Reagents:
2-bromo-4-methylpropiophenone (BK4) - 5 kg;
n-methyl-2-pyrrolidone (NMP) - 20 L;
Methyl amine 40% aq.soln - 8 L;
Benzene - 15 L;
Acetone - 30 L;
Hydrochloric acid con.aq.soln ~ 1,5 L.
Synthesis:
1. 5 kg 2-bromo-4-methylpropiophenone (BK4) added to the reactor or have calculated amount of crude BK4 after halogenation reactions.
2. 20 liters n-methyl-2-pyrrolidone poured, start stirring and heating to 40 *C.
3. Upon reaching 40 *C within the mixture, pour 8 liters methyl amine 40% aq.soln and continue stirring 20 minutes.
4. Next, we pour 20 liters of clean cold water, stirring a few minutes.
5. Pour 15-20 liters benzene or other suitable extractor, stirring a few minutes.
6. Stop stirring, waiting for the separation of the mixture into two layers.
7. The bottom aqueous layer was drained through the bottom valve of the reactor.
8. 20 liters of ice acetone was poured and add hydrochloric acid with stirring to pH - 5
9. Overload the mixture in the freezer.
10. Filter on the nutshe-filter, dry.
Notes:
NMP can be replaced by DMSO, DMF, Sulfolane.
Hello William,
Changing 2-bromo-4-methylpropiophenone with 2
bromo, 3-chloropropiophenone will get me 3cmc. Many thanks!
Exactly
Reaction scheme:
View attachment 1218
Reagents:
2-bromo-4-methylpropiophenone (BK4) - 5 kg;
n-methyl-2-pyrrolidone (NMP) - 20 L;
Methyl amine 40% aq.soln - 8 L;
Benzene - 15 L;
Acetone - 30 L;
Hydrochloric acid con.aq.soln ~ 1,5 L.
Synthesis:
1. 5 kg 2-bromo-4-methylpropiophenone (BK4) added to the reactor or have calculated amount of crude BK4 after halogenation reactions.
2. 20 liters n-methyl-2-pyrrolidone poured, start stirring and heating to 40 *C.
3. Upon reaching 40 *C within the mixture, pour 8 liters methyl amine 40% aq.soln and continue stirring 20 minutes.
4. Next, we pour 20 liters of clean cold water, stirring a few minutes.
5. Pour 15-20 liters benzene or other suitable extractor, stirring a few minutes.
6. Stop stirring, waiting for the separation of the mixture into two layers.
7. The bottom aqueous layer was drained through the bottom valve of the reactor.
8. 20 liters of ice acetone was poured and add hydrochloric acid with stirring to pH - 5
9. Overload the mixture in the freezer.
10. Filter on the nutshe-filter, dry.
Notes:
NMP can be replaced by DMSO, DMF, Sulfolane.
What step should I undergo if I still have to react the bromine with the 4-methylpropiophenone. In what quantity for this scale? I also need benzene for that, right?
small portions making sure the mixture does not exceed 60 degrees?
yes, but your water will turn to icepoint 4 mentions cold pure water, can it be cooled with dry ice to these 3-5 degrees C?
Yes, but you don't need to use so cold acetone. -5-10 *C Is enoughpoint 8 mentions ice-cold acetone, can I add a large amount of dry ice to it to cool it to -30 / -50 degrees C?
The purpose is crystallization. Low temperature helps to form crystals of mephedrone from solution.point 9 mentions putting the whole thing in the freezer, what is the purpose of this and is it necessary?
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