HRID716727

反应详情

EQUATION

反应方程式

HRID 716727 的结构方程式

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

  1. temperatureThe reaction temperature was maintained for 14-20 h
  2. customUpon completion of the reaction
  3. temperaturethe reaction mixture was cooled to 50-80° C.
  4. customacetic anhydride was recovered at 50-80° C. at reduced pressure
  5. extractionthe crude product was extracted with dichloromethane (500 mL)
  6. customThe dichloromethane layer was recovered completely
  7. customto obtain the product