反应详情

38.8 g of potassium carbonate was added to a solution of 50 g of 5-dimethylamino-2,3,4,5-tetrahydro-1H-benzoazepine dissolved in 400 ml of acetone and 200 ml of water. To the mixture was added 66.5 g of 4-[2-(2-chloro-phenyl)acetylamino]benzoyl chloride with ice-cooling and stirring. The mixture was stirred overnight at room temperature. The reaction mixture was mixed with water, followed by extraction with dichloromethane. The dichloromethane layer was dried over magnesium sulfate and then subjected to vacuum distillation to remove the solvent. The residue was purified by silica gel column chromatography and then recrystallized from methanol to obtain 99.3 g of 5-dimethylamino-1-{4-[2-(2-chlorophenyl)acetylamino]benzoyl}-2,3,4,5-tetrahydro-1H-benzoazepine.

1. temperaturecooling
2. stirringThe mixture was stirred overnight at room temperature
3. extractionfollowed by extraction with dichloromethane
4. dry with materialThe dichloromethane layer was dried over magnesium sulfate
5. distillationsubjected to vacuum distillation
6. customto remove the solvent
7. customThe residue was purified by silica gel column chromatography
8. customrecrystallized from methanol