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 200 g of acetic acid was dissolved 30 g of bis(4-butoxyphenyl) sulfide obtained in Synthesis Example 1-17. While the solution was maintained at an internal temperature of 30° C., 8.8 g of 35 wt % aqueous hydrogen peroxide was added dropwise. The reaction solution was aged at room temperature for 12 hours, after which under ice cooling, a mixture of 0.9 g sodium thiosulfate pentahydrate and 30 g water was added dropwise to quench the reaction. The solution was combined with 200 g of methylene chloride and 50 g of water for extraction. The organic layer was separated, washed with water, and concentrated in vacuum. On subsequent purification by silica gel chromatography, 28 g of the target compound, bis(4-butoxyphenyl) sulfoxide was obtained as amorphous solid. Yield 90%.
WORKUP
后处理
- customobtained in Synthesis Example 1-17
- additionwas added dropwise
- additionwas added dropwise
- customto quench
- customthe reaction
- extractionThe solution was combined with 200 g of methylene chloride and 50 g of water for extraction
- customThe organic layer was separated
- washwashed with water
- concentrationconcentrated in vacuum
- customOn subsequent purification by silica gel chromatography, 28 g of the target compound