HRID5207
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 a solution of 5.0 g p-(3,5-difluorophenoxy)phenol in 50 mg of carbon tetrachloride, there were added dropwise 2.45 of tert-butylhypochlorous acid with stirring and ice-cooling, and stirring was continued at room temperature for 5 hours. The reaction mixture was concentrated and extracted with 200 ml of ethyl acetate. The extract was washed with 5% aqueous solution of sodium bicarbonate, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography to give 5.31 g of 2-chloro-4-(3,5-difluorophenoxy)phenol. Yield, 92%. nD25 : 1.5639
WORKUP
后处理
- temperatureice-cooling
- stirringstirring
- concentrationThe reaction mixture was concentrated
- extractionextracted with 200 ml of ethyl acetate
- washThe extract was washed with 5% aqueous solution of sodium bicarbonate
- dry with materialdried over anhydrous magnesium sulfate
- concentrationconcentrated under reduced pressure