HRID402917

反应详情

EQUATION

反应方程式

HRID 402917 的结构方程式

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 5-bromo-2-(1-carboxy-ethoxy)-benzoic acid (31.2 g, 108 mmol), acetic anhydride (216 mL) and anhydrous sodium acetate (21.8 g, 266 mmol) is heated under reflux (150° C.) for 4 h. After cooling to room temperature the reaction mixture is carefully quenched with ice-cold water (500 mL). A white precipitate is formed which is collected by suction filtration, thoroughly washed with water and dried in vacuo at 45° C. to afford the title compound as a white powder (19.0 g, 70.6 mmol, 65%). MS (ES+): 269 (M(C11H979BrO3)+H)+.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureAfter cooling to room temperature the reaction mixture
  3. customis carefully quenched with ice-cold water (500 mL)
  4. customA white precipitate is formed which
  5. filtrationis collected by suction filtration
  6. washthoroughly washed with water
  7. customdried in vacuo at 45° C.