HRID852060

反应详情

EQUATION

反应方程式

HRID 852060 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 2,4-dichlorophenoxy acetic acid (15.0 g) in tetrahydrofuran (300 mL) was added dropwise 1.0M borane-tetrahydrofuran complex/tetrahydrofuran solution (96 mL) under ice-cooling over 1.5 hours. The reaction solution was stirred at room temperature for 22 hours. After the reaction solution was concentrated, the residue was diluted with saturated aqueous ammonium chloride solution and ethyl acetate. The organic layer was washed with saturated ammonium chloride, saturated aqueous sodium hydrogencarbonate solution (×2) and saturated ammonium chloride, dried over anhydrous sodium sulfate and then concentrated, to give the title compound as a colorless oil (14 g).

WORKUP

后处理

  1. temperaturecooling over 1.5 hours
  2. concentrationAfter the reaction solution was concentrated
  3. additionthe residue was diluted with saturated aqueous ammonium chloride solution and ethyl acetate
  4. washThe organic layer was washed with saturated ammonium chloride, saturated aqueous sodium hydrogencarbonate solution (×2) and saturated ammonium chloride
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated