反应详情

温度

150 °C

A solution of Intermediate 71 (104 mg) in dimethyl sulfoxide (2 ml) was added with cesium fluoride (284 mg, Wako Pure Chemical Industries) and stirred at 150° C. for 8 hours. The reaction mixture was cooled to room temperature and then filtered through Celite. The residue was added with water (20 ml), extracted with ethyl acetate (20 ml) and washed twice with saturated brine (10 ml for each time). The organic layer was dried over anhydrous sodium sulfate, and then the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=3:1) to obtain the title compound (21.1 mg).

1. temperatureThe reaction mixture was cooled to room temperature
2. filtrationfiltered through Celite
3. additionThe residue was added with water (20 ml)
4. extractionextracted with ethyl acetate (20 ml)
5. washwashed twice with saturated brine (10 ml for each time)
6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
7. customthe solvent was evaporated under reduced pressure
8. customThe residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=3:1)