反应详情

To 320 ml of dichloromethane were dissolved 20.2 g (0.1 mol) of diphenylsulfoxide and 19.6 g (0.1 mol) of xanthene-9-one, and 28.2 g (0.1 mol) of trifluoromethanesulfonic anhydride was added dropwise thereto at −70 to −60° C., followed by gradually warming to room temperature and reacting with stirring for 4 hours. After completion of the reaction, the obtained reaction solution was washed with water (160 ml×4 times) and concentrated under reduced pressure, followed by purifying the obtained crude product with column chromatography to obtain 30.7 g of objective substance as pale brown glassy substance (yield: 58%).

1. additionwas added dropwise
2. customat −70 to −60° C.
3. customAfter completion of the reaction
4. customthe obtained reaction solution
5. washwas washed with water (160 ml×4 times)
6. concentrationconcentrated under reduced pressure
7. customby purifying the
8. customobtained crude product with column chromatography
9. customto obtain 30.7 g of objective substance as pale brown glassy substance (yield: 58%)