反应 #1435732

反应方程式

5-hydroxy-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine

N,N-diethylaniline

phosphorus oxychloride

→

5-chloro-6-(2-chloro-6-fluorophenyl)-7-methylimidazo[1,2-a]pyrimidine

反应条件

后处理

1. 1
   温度was refluxed
2. 2
   温度under heating for 26 hours
3. 3
   浓缩The reaction mixture was concentrated
4. 4
   workup.ADDITIONdichloromethane and aqueous saturated sodium bicarbonate solution were added to the residue
5. 5
   洗涤The separated organic layer was washed with water
6. 6
   干燥dried over sodium sulfate
7. 7
   浓缩concentrated

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.

来源