HRID1172034
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwas added dropwise
- customat −70 to −60° C.
- customAfter completion of the reaction
- customthe obtained reaction solution
- washwas washed with water (160 ml×4 times)
- concentrationconcentrated under reduced pressure
- customThe obtained crude product
- customwas purified by column chromatography
- customto obtain 38.6 g of objective substance as yellow glassy substance (yield: 64%)