HRID5207

反应详情

EQUATION

反应方程式

HRID 5207 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureice-cooling
  2. stirringstirring
  3. concentrationThe reaction mixture was concentrated
  4. extractionextracted with 200 ml of ethyl acetate
  5. washThe extract was washed with 5% aqueous solution of sodium bicarbonate
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure