HRID128612
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
PROCEDURE
实验过程
A mixture of sodium methoxide (prepared from sodium metal) (10.2 g) and methanol (175 ml), 3-hydroxy-2-methylpyridine (43.0 g) phenyltrimethylammonium chloride (81.9 g) and DMF (400 ml) was boiled under reflux with stirring for 5 hours under nitrogen. The mixture was filtered and distilled. The fraction boiling at 167°-195° C. was collected and purified by flash chromatography on silica using dichloromethane and then IMS as the mobile phase to give 3-methoxy-2-methylpyridine which was used without further purification.
WORKUP
后处理
- temperatureunder reflux
- filtrationThe mixture was filtered
- distillationdistilled
- customThe fraction boiling at 167°-195° C. was collected
- custompurified by flash chromatography on silica