反应详情

With stirring at room temperature, the compound (3.30 g, 13.9 mmol) obtained in step C, triethylsilane (4.4 ml, (27.8 mmol) and boron trifluoride-diethyl ether complex (3.4 ml, 27.8 mmol) dissolved in 1,2-dichloroethane (20 ml) were added to 1,2-dichloroethane (90 ml), and the mixture was stirred at 83° C. for 1 hr. After cooling to room temperature, the reaction mixture was diluted with water, and extracted with dichloromethane. The organic layer was washed with diluted aqueous sodium hydroxide solution, diluted hydrochloric acid and saturated brine, and dried over anhydrous magnesium sulfate. The solution was concentrated under reduced pressure to give the title compound (2.76 g, yield 91%) as a pale-yellow solid.

1. stirringthe mixture was stirred at 83° C. for 1 hr
2. temperatureAfter cooling to room temperature
3. extractionextracted with dichloromethane
4. washThe organic layer was washed with diluted aqueous sodium hydroxide solution, diluted hydrochloric acid and saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. concentrationThe solution was concentrated under reduced pressure