HRID1459664

反应详情

EQUATION

反应方程式

HRID 1459664 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.2 g (15 mmol) of 2-amino-5-fluorobenzenethiol was dissolved in 30 ml of dimethylformamide and 2.5 g (12 mmol) of 1-chloro-2,6-dinitrobenzene was added thereto. The resulting mixture was stirred at room temperature. After 12 hours, 2.6 ml of N,N-diisopropylethylamine was added thereto and the mixture was heated at 80° C. for 2 hours. After cooling, the reaction mixture was poured into a saturated aqueous solution of ammonium chloride and extracted with ethyl acetate. After concentrating, the residue was purified by silica gel column chromatography. Thus 1.2 g of the title compound was obtained.

WORKUP

后处理

  1. temperaturethe mixture was heated at 80° C. for 2 hours
  2. temperatureAfter cooling
  3. extractionextracted with ethyl acetate
  4. concentrationAfter concentrating
  5. customthe residue was purified by silica gel column chromatography