HRID216698
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureis heated
- temperatureAfter cooling to room temperature the reaction mixture
- customis carefully quenched with ice-cold water (500 mL)
- customA white precipitate is formed which
- filtrationis collected by suction filtration
- washthoroughly washed with water
- customdried in vacuo at 45° C.