HRID379114

反应详情

EQUATION

反应方程式

HRID 379114 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred mixture of 4-[(3-bromophenyl)amino]-8-methyl-6-nitro-quinoline-3-carbonitrile (15.3 g, 40 mmol), 0.37 g (3 mmol) of dimethylaminopyridine, 40 ml of acetic anhydride, and 80 ml of pyridine was refluxed for 3 h and concentrated at 50° C. under vacuum. The residue was stirred with methylene chloride and 0.1 N HCl. After filtration through Celite, the organic layer was washed with water, dried and concentrated. The residue was subjected to chromatography on silica gel with 1% acetic acid in methylene chloride to give 11.2 g of an amber glass, NMR (CDCl3) d 2.29 (N-acetyl group).

WORKUP

后处理

  1. temperaturewas refluxed for 3 h
  2. concentrationconcentrated at 50° C. under vacuum
  3. filtrationAfter filtration through Celite
  4. washthe organic layer was washed with water
  5. customdried
  6. concentrationconcentrated