反应详情

A mixture of 1B (6.93 g, 30 mmol), acetic anhydride (3.5 ml, 36 mmol) and pyridine (15 ml) is heated under reflux with stirring for 16 hours. The reaction mixture is diluted with water and ethyl acetate. The organic phase is acidified with dilute hydrochloric acid and washed with water twice. The organic phase is concentrated in vacuo and the residue is purified by flash chromatography (dichloromethane:methanol, 9:1 v/v) yielding the pure product as a yellow oil, 7.4 g, (90.3%).

1. temperatureis heated
2. temperatureunder reflux
3. washwashed with water twice
4. concentrationThe organic phase is concentrated in vacuo
5. customthe residue is purified by flash chromatography (dichloromethane:methanol, 9:1 v/v)