HRID1172034

反应详情

EQUATION

反应方程式

HRID 1172034 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 320 ml of dichloromethane were dissolved 20.2 g (0.1 mol) of diphenylsulfoxide and 26.8 g (0.1 mol) of 2,4-diethylthioxanthene-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. The obtained crude product was purified by column chromatography to obtain 38.6 g of objective substance as yellow glassy substance (yield: 64%).

WORKUP

后处理

  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. customThe obtained crude product
  8. customwas purified by column chromatography
  9. customto obtain 38.6 g of objective substance as yellow glassy substance (yield: 64%)