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
In 120 g of acetic acid was dissolved 17.1 g of phenyl 4-(2,2,2-trifluoroethoxy)phenyl sulfide obtained in Synthesis Example 1-13. While the solution was maintained at an internal temperature of 30° C., 5.8 g of 35 wt % aqueous hydrogen peroxide was added dropwise. The reaction solution was aged at room temperature for 18 hours, after which under ice cooling, a mixture of 0.5 g sodium thiosulfate pentahydrate and 15 g water was added dropwise to quench the reaction. The solution was combined with 100 g of toluene, 50 g of ethyl acetate, and 50 g of water. The organic layer was separated, washed with water, and concentrated in vacuum. This was followed by crystallization from hexane, filtration, and drying. There was obtained 17.9 g of the target compound, phenyl 4-(2,2,2-trifluoroethoxy)phenyl sulfoxide as white crystals. Yield 99%.
WORKUP
后处理
- customobtained in Synthesis Example 1-13
- additionwas added dropwise
- additionwas added dropwise
- customto quench
- customthe reaction
- customThe organic layer was separated
- washwashed with water
- concentrationconcentrated in vacuum
- customThis was followed by crystallization from hexane, filtration
- customdrying