HRID902879
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationThe reaction mixture was concentrated under reduced pressure
- dissolutionthe resultant residue was dissolved in acetic acid (50 ml)
- additionAcetic anhydride (5.0 ml) was added to the solution
- temperaturethe mixture was heated
- temperatureunder reflux for 16 hours
- distillationThe solvent was distilled off under reduced pressure, and ethanol
- additionwas added to the residue
- filtrationCrystals deposited were collected by filtration
- washwashed