反应详情

97 mg (0.57 mmol) of thionyl chloride were added to a solution of 200 mg (0.52 mmol) of the compound from Example 49A in 1 ml of dichloromethane. The mixture was stirred under reflux for 1 h. For work-up, the dichloromethane was removed under reduced pressure, and once more dichloromethane was added to the residue and the mixture was concentrated. The residue was initially charged in 5 ml of dichloromethane, and 78 mg (0.78 mmol) of triethylamine and 97 mg (0.57 mmol) of 2-amino-1-phenylethanone were then added. The reaction mixture was stirred at room temperature for 3 h. For work-up, water was added to the mixture, and the organic phase was separated off and washed repeatedly with saturated aqueous sodium chloride solution. The organic phase was dried over magnesium sulphate and evaporated to dryness under reduced pressure. Yield: 300 mg (62% of theory, 70% pure)

1. temperatureunder reflux for 1 h
2. customFor work-up, the dichloromethane was removed under reduced pressure, and once more dichloromethane
3. additionwas added to the residue
4. concentrationthe mixture was concentrated
5. additionThe residue was initially charged in 5 ml of dichloromethane
6. stirringThe reaction mixture was stirred at room temperature for 3 h
7. customthe organic phase was separated off
8. washwashed repeatedly with saturated aqueous sodium chloride solution
9. dry with materialThe organic phase was dried over magnesium sulphate
10. customevaporated to dryness under reduced pressure