HRID2239301

反应详情

EQUATION

反应方程式

HRID 2239301 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A mixture of methyl 3-(3,5-difluorophenoxy)propanoate (11.6 g, 53.7 mmol, STEP 6) and trifluoromethanesulfonic acid (23.2 mL, 2.0 mL/g of substrate) was stirred at 80° C. for 2 hours. After cooling to room temperature, the reaction mixture was diluted with water (120 mL), and extracted with toluene (120 mL). The organic layer was washed successively with aqueous solution of potassium carbonate (50 mL), water (50 mL), and dried over magnesium sulfate. The organic mixture was concentrated in vacuum to afford the title compound (8.75 g, 88%) as a white solid, which was used in the next step without further purification.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature
  2. extractionextracted with toluene (120 mL)
  3. washThe organic layer was washed successively with aqueous solution of potassium carbonate (50 mL), water (50 mL)
  4. dry with materialdried over magnesium sulfate
  5. concentrationThe organic mixture was concentrated in vacuum