HRID1488943

反应详情

EQUATION

反应方程式

HRID 1488943 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
10 °C

PROCEDURE

实验过程

To a solution of 52.7 g (0.80 mol) of potassium hydroxide (85%) in 300 ml of ethanol and 30 ml of water 59.4 g (0.15 mol) of 2,3-dibromo-3-(3,4-dimethoxyphenyl)propionic acid ethyl ester are added at 25° C. over 10 minutes. The mixture is stirred under reflux for 2.5 hours. The solvent is evaporated, the residue dissolved in 200 ml of water and, with cooling to 10° C., the solution acidified with 2N hydrochloric acid. The resulting crystals are filtered off, washed with water and recrystallized from methanol/water.

WORKUP

后处理

  1. temperatureunder reflux for 2.5 hours
  2. customThe solvent is evaporated
  3. dissolutionthe residue dissolved in 200 ml of water
  4. filtrationThe resulting crystals are filtered off
  5. washwashed with water
  6. customrecrystallized from methanol/water