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I've tried this synthesis and gotten yields ranging from 30% 45%. Sharing in case it might be helful to others. Vice versa, other people might know changes to this synthesis for higher yields.
Improvements are always welcome
Needed:
100 g 2-bromo-4-methylpropiophenone
500 ml DCM
200 ml Methylamine 40% aqua solution
60 ml HCI 30÷ aqua solution
550 ml Acetone
2 L Deminiralised water
PH measuring Strips
1 L IPA
Equipment:
Round bottom flask 2 L
Hotplate
Measuring cups 1 L
Crystallization dish
Vacuum pump
Buchner flask
1. Add 100 g 2-bromo-4-methylpropiophenone to 500 ml DCM and let it dissolve.
2. Add 200 ml methylamine in 4 portions
3. After 30 mins, put on hotplate and stir.
4. Temperature 32-36 C for 4 hours, or 40 C for 2 hours.
5. Rinse in measuring cup with demi-water until there is no methylamine smell left. Stir or shake after adding.
6. Add an ice cold solution of acetone/HCI 550ml/60ml, or add ice cold acetone and add HCI after.
7. Measure the PH, should be 6.
7. Put the 4-MMC freebase in freezer for 12h
8. Rinse with ice cold acetone trough buchner filter.
9. If you have obtained dry 4-MMC prepare a solution of 50/50 demi-water and IPA. Add 1g per 2-3 ml solvent. Boil until 4-MMC (Not longer than needed, aprox. 1-3 min.). Pour into a crystallization dish. When crystallization stops at room temperature, put the dish in the fridge. Put in freezer after and you will be left with nice looking crystals.
Improvements are always welcome
Needed:
100 g 2-bromo-4-methylpropiophenone
500 ml DCM
200 ml Methylamine 40% aqua solution
60 ml HCI 30÷ aqua solution
550 ml Acetone
2 L Deminiralised water
PH measuring Strips
1 L IPA
Equipment:
Round bottom flask 2 L
Hotplate
Measuring cups 1 L
Crystallization dish
Vacuum pump
Buchner flask
1. Add 100 g 2-bromo-4-methylpropiophenone to 500 ml DCM and let it dissolve.
2. Add 200 ml methylamine in 4 portions
3. After 30 mins, put on hotplate and stir.
4. Temperature 32-36 C for 4 hours, or 40 C for 2 hours.
5. Rinse in measuring cup with demi-water until there is no methylamine smell left. Stir or shake after adding.
6. Add an ice cold solution of acetone/HCI 550ml/60ml, or add ice cold acetone and add HCI after.
7. Measure the PH, should be 6.
7. Put the 4-MMC freebase in freezer for 12h
8. Rinse with ice cold acetone trough buchner filter.
9. If you have obtained dry 4-MMC prepare a solution of 50/50 demi-water and IPA. Add 1g per 2-3 ml solvent. Boil until 4-MMC (Not longer than needed, aprox. 1-3 min.). Pour into a crystallization dish. When crystallization stops at room temperature, put the dish in the fridge. Put in freezer after and you will be left with nice looking crystals.