HRID1392773

反应详情

EQUATION

反应方程式

HRID 1392773 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl chlorooxoacetate (2.0 ml) was added to a solution of 2-amino-5-chlorobenzamide (2.50 g) in pyridine (15 ml), and the mixture was stirred at room temperature for 18 hours. The reaction mixture was concentrated under reduced pressure, and the resultant residue was dissolved in acetic acid (50 ml). Acetic anhydride (5.0 ml) was added to the solution, and the mixture was heated under reflux for 16 hours. The solvent was distilled off under reduced pressure, and ethanol was added to the residue. Crystals deposited were collected by filtration and washed to obtain the title compound (2.71 g).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. dissolutionthe resultant residue was dissolved in acetic acid (50 ml)
  3. additionAcetic anhydride (5.0 ml) was added to the solution
  4. temperaturethe mixture was heated
  5. temperatureunder reflux for 16 hours
  6. distillationThe solvent was distilled off under reduced pressure, and ethanol
  7. additionwas added to the residue
  8. filtrationCrystals deposited were collected by filtration
  9. washwashed