反应详情

A solution of diethylamino sulfurtrifluoride (DAST), (9.34 g, 1.75 eq ) in 10 ml of dichloromethane was added drop wise to the solution of 14 (12.3 g) and antimony (III) chloride (0.23 g, 0.03 eq ) in 150 ml of dichloromethane (anhydrous) at −5° C., and the reaction mixture was warmed up to room temperature overnight. A cold saturated solution of sodium bicarbonate (80 ml) was added and stirred for 30 min and extracted with dichloromethane (100 ml×2). The organic layer was washed with a 10% solution of sodium bicarbonate and with brine (50 ml) and dried over sodium sulfate. After purification, via a column, 10.7 g of the desired product (as a heavy oil) was obtained.

1. extractionextracted with dichloromethane (100 ml×2)
2. washThe organic layer was washed with a 10% solution of sodium bicarbonate and with brine (50 ml)
3. dry with materialdried over sodium sulfate
4. customAfter purification