HRID1348550
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperaturewas refluxed
- temperatureunder heating for 26 hours
- concentrationThe reaction mixture was concentrated
- additiondichloromethane and aqueous saturated sodium bicarbonate solution were added to the residue
- washThe separated organic layer was washed with water
- dry with materialdried over sodium sulfate
- concentrationconcentrated