HRID420453

反应详情

EQUATION

反应方程式

HRID 420453 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Suspending 3.0 g (15 mmol) of 4-bromobenzoic acid into 30 milliliter of 1,2-dichloroethane, adding 2.7 g (23 mmol) of thionyl chloride and 3 drops of N,N-dimethylformamide, the resultant solution was stirred with heating at the temperature of about 50° C. for 1 hour and 30 minutes until benzoic acid as the material disappeared. After completion of the reaction, removing the solvent and excess thionyl chloride by distillation, dissolving the resultant acid chloride into 30 milliliter of N-methylpyrrolidone, adding 2.8 g (15 mmol) of N-phenyl-1,2-phenylenediamine, the resultant solution was stirred at room temperature for a night. After completion of the reaction, adding water and filtering the precipitated solid, further washing with water and by drying under reduced pressure, 5.2 g of 4-bromo-N-(2-phenylamino-phenyl)-benzamide was obtained.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. customremoving the solvent and excess thionyl chloride
  3. distillationby distillation
  4. dissolutiondissolving the resultant acid chloride into 30 milliliter of N-methylpyrrolidone
  5. customAfter completion of the reaction
  6. filtrationfiltering the precipitated solid
  7. washfurther washing with water
  8. customby drying under reduced pressure