HRID1753674

反应详情

EQUATION

反应方程式

HRID 1753674 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

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

  1. customobtained in Synthesis Example 1-13
  2. additionwas added dropwise
  3. additionwas added dropwise
  4. customto quench
  5. customthe reaction
  6. customThe organic layer was separated
  7. washwashed with water
  8. concentrationconcentrated in vacuum
  9. customThis was followed by crystallization from hexane, filtration
  10. customdrying