HRID1392364

反应详情

EQUATION

反应方程式

HRID 1392364 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

Part A; To 4-bromobenzaldehyde (25 gram, 0.135 mol) is successively added 2,4-dichlorophenylacetic acid (27.7 gram, 0.135 mol), acetic anhydride (100 mL) and triethylamine (19 mL, 0.136 mol) and the resulting mixture is heated at reflux temperature for 90 minutes. The reaction mixture is cooled to 110° C. and water (100 mL) is slowly added. The resulting mixture is allowed to attain room temperature and ethyl acetate is added. The ethyl acetate layer is twice washed with water, dried over MgSO4, filtered and concentrated in vacuo. The resulting oil is crystallised from diisopropyl ether to give 3-(4-bromophenyl)-2-(2,4-dichlorophenyl)acrylic acid as a white solid (26.55 gram, 53% yield).

WORKUP

后处理

  1. temperaturethe resulting mixture is heated
  2. temperatureat reflux temperature for 90 minutes
  3. customto attain room temperature
  4. washThe ethyl acetate layer is twice washed with water
  5. dry with materialdried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe resulting oil is crystallised from diisopropyl ether