HRID716727
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
- 135 °C
PROCEDURE
实验过程
To acetic anhydride (300 mL) was added 2-(carboxymethoxy)benzoic acid (7) (100 g, 0.510 mol) at ambient temperature and heated to 130-140° C. The reaction temperature was maintained for 14-20 h under stirring. The progress of the reaction was monitored by the HPLC analysis. Upon completion of the reaction, the reaction mixture was cooled to 50-80° C., acetic anhydride was recovered at 50-80° C. at reduced pressure and the crude product was extracted with dichloromethane (500 mL). The dichloromethane layer was recovered completely to obtain the product meeting the desired specifications. Yield—76-85%.
WORKUP
后处理
- temperatureThe reaction temperature was maintained for 14-20 h
- customUpon completion of the reaction
- temperaturethe reaction mixture was cooled to 50-80° C.
- customacetic anhydride was recovered at 50-80° C. at reduced pressure
- extractionthe crude product was extracted with dichloromethane (500 mL)
- customThe dichloromethane layer was recovered completely
- customto obtain the product