HRID1857620

反应详情

EQUATION

反应方程式

HRID 1857620 的结构方程式

PROCEDURE

实验过程

To a suspension of 2-amino-4-chloro-5-nitrobenzoic acid methyl ester (989 mg in 15 mL of dry 1,2-dichloroethane) was added a solution of (3,5-dimethylphenyl)acetyl chloride (860 mg in 5 mL dry 1,2-dichloroethane) and the mixture heated at reflux on an oil bath. After 18 hours, an additional portion of (3,5-dimethylphenyl)acetyl chloride (274 mg in 1.5 mL dry 1,2-dichloroethane) was added and the mixture heated at reflux for an additional 5 hours. At this time the reaction was cooled and the solvent removed in vacuo. Recrystallization of the crude product from methanol gave the title compound (1.17 g).

WORKUP

后处理

  1. temperaturethe mixture heated
  2. temperatureat reflux on an oil bath
  3. temperaturethe mixture heated
  4. temperatureat reflux for an additional 5 hours
  5. temperatureAt this time the reaction was cooled
  6. customthe solvent removed in vacuo
  7. customRecrystallization of the crude product from methanol