HRID1348550

反应详情

EQUATION

反应方程式

HRID 1348550 的结构方程式

PROCEDURE

实验过程

A mixture of 0.16 g of 5-hydroxy-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine, 0.20 g of N,N-diethylaniline and 2 ml of phosphorus oxychloride was refluxed under heating for 26 hours. The reaction mixture was concentrated, and dichloromethane and aqueous saturated sodium bicarbonate solution were added to the residue. The separated organic layer was washed with water, dried over sodium sulfate and concentrated. The residue was subjected to silica gel chromatography to give 45mg of 5-chloro-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine.

WORKUP

后处理

  1. temperaturewas refluxed
  2. temperatureunder heating for 26 hours
  3. concentrationThe reaction mixture was concentrated
  4. additiondichloromethane and aqueous saturated sodium bicarbonate solution were added to the residue
  5. washThe separated organic layer was washed with water
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated