HRID216697

反应详情

EQUATION

反应方程式

HRID 216697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
75 °C

PROCEDURE

实验过程

A suspension of acetic acid 5-bromo-2-methyl-benzofuran-3-yl ester (18.9 g, 70.4 mmol) in methanol (232 mL) and a I M aqueous HCl solution (44 mL) is heated under reflux (75° C.) for 7 h. After cooling to room temperature the reaction mixture is concentrated by rotary evaporation. The residue is diluted with water and extracted three times with diethyl ether. The combined organic layers are washed with water, brine, dried over Na2SO4, filtered and concentrated at reduced pressure to afford the title compound as a yellow oil (14.7 g, 64.7 mmol, 92%). MS (ES+): 227 (M(C9H779BrO2)+H)+.

WORKUP

后处理

  1. temperatureAfter cooling to room temperature the reaction mixture
  2. concentrationis concentrated by rotary evaporation
  3. additionThe residue is diluted with water
  4. extractionextracted three times with diethyl ether
  5. washThe combined organic layers are washed with water, brine
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated at reduced pressure