反应详情

A mixture of 6A (9.8 g, 34.1 mmol), water (40 ml), ethanol (80 ml) and sodium hydroxide (2.7 g, 68.3 mmol) is heated under reflux with stirring for 42 hours. The reaction mixture is diluted with water (80 ml), acidified with concentrated hydrochloric acid and extracted with dichloromethane. The organic phase is separated and concentrated. The solid material is collected by filtration, washed with water and dried yielding off-white crystals, 5.4 g (61%), mp 81-83° C.

1. temperatureis heated
2. temperatureunder reflux
3. extractionextracted with dichloromethane
4. customThe organic phase is separated
5. concentrationconcentrated
6. filtrationThe solid material is collected by filtration
7. washwashed with water
8. customdried
9. customyielding off-white crystals, 5.4 g (61%), mp 81-83° C.