反応 #1435732

反応方程式

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

反応条件

後処理

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

実験手順

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.

出典