HRID1440327

反应详情

EQUATION

反应方程式

HRID 1440327 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Added to 500 g (4.2 mol) of thionyl chloride were 110 g (0.58 mol) of 3-phenylisoxazole-5-carboxylic acid prepared above in the procedure (2), followed by the further addition of 2 ml of dimethylformamide. The resulting mixture was heated under reflux for 3 hours. After completion of the reaction, thionyl chloride was distilled off under reduced pressure, followed by the addition of 500 ml of benzene. When the mixture thus obtained was distilled under reduced pressure, the title compound, i.e., 3-phenylisoxazole-5-carboxylic acid chloride was obtained as a solid. It was provided for the next step without purification.

WORKUP

后处理

  1. customprepared above in the procedure (2)
  2. temperatureThe resulting mixture was heated
  3. temperatureunder reflux for 3 hours
  4. distillationwas distilled off under reduced pressure
  5. additionfollowed by the addition of 500 ml of benzene
  6. customWhen the mixture thus obtained
  7. distillationwas distilled under reduced pressure