HRID651430
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 110 °C
PROCEDURE
实验过程
5.0 g of 2,6-dichloro-4-pyridinemethanol and 2.5 ml of pyridine were suspended in 10 ml of toluene, and the suspension was cooled in a salt-ice bath. To this, 2.7 ml of thionyl chloride were added dropwise for 1 hour, and subsequently the reacted solution was stirred at 110° C. for 3 hours. After cooling, water was added to the solution, and extraction was conducted using diethyl ether. The organic phase was washed with water, and was dried by adding sodium sulfate. The solvent was removed by evaporation, and the residue was purified by silica gel column chromatography to obtain 5.0 g of 2,6-dichloro-4-chloromethylpyridine.
WORKUP
后处理
- temperaturethe suspension was cooled in a salt-ice bath
- temperatureAfter cooling
- washThe organic phase was washed with water
- customwas dried
- additionby adding sodium sulfate
- customThe solvent was removed by evaporation
- customthe residue was purified by silica gel column chromatography