Dimethylformamide dimethyl acetal → 3'-Chloro-3-dimethylamino-2-methylacrylophenone
Reaktionsgleichung
[Cl:1][C:2]1[CH:3]=[C:4]([C:8](=[O:11])[CH2:9][CH3:10])[CH:5]=[CH:6][CH:7]=1.CO[CH:14](OC)[N:15]([CH3:17])[CH3:16]>>[Cl:1][C:2]1[CH:3]=[C:4]([C:8](=[O:11])[C:9]([CH3:10])=[CH:14][N:15]([CH3:16])[CH3:17])[CH:5]=[CH:6][CH:7]=1Komponenten
3
Versuchsvorschrift
A mixture of 75.0 g of m-chloropropiophenone and 200 ml of N,N-dimethylformamide dimethyl acetal was stirred and heated at reflux for 16 hours. The mixture was evaporated in vacuo to give a black oil. The oil was subjected to Kugelrohr distillation at 0.5 mm of mercury and the fraction that boils at 110° C. was removed. The residue from the distillation was collected to give 35.0 g of 3'-chloro-3-dimethylamino-2-methylacrylophenone as a black oil.
Aufarbeitung
- temperatureheated
- temperatureat reflux for 16 hours
- customThe mixture was evaporated in vacuo
- customto give a black oil