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
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
2-(3,5-Dichlorophenyl)-3,3,3-trifluoroprop-1-en-1-yl phenyl sulfide (1.00 g, 94% purity, 2.69 mmol) was dissolved in glacial acetic acid (5 mL) and hydrogen peroxide (0.54 mL, 35% in water, 6:19 mml) was added in one portion. The reaction mixture was heated to 50° C. and stirred for three hours at that temperature. After cooling, toluene and water were added and the phases were separated. The aqueous phase was extracted with toluene and the combined organic phases were washed two times with saturated sodium bicarbonate solution and once with sodium metabisulfite solution (30% w/w solution in water). Drying over sodium sulfate, filtration and evaporation yielded 2-(3,5-dichlorophenyl)-3,3,3-trifluoroprop-1-en-1-yl phenyl sulfoxide (950 mg, 94% purity, 91% yield, E/Z=93/7).
WORKUP
后处理
- temperatureAfter cooling
- customthe phases were separated
- extractionThe aqueous phase was extracted with toluene
- washthe combined organic phases were washed two times with saturated sodium bicarbonate solution
- dry with materialDrying over sodium sulfate, filtration and evaporation