HRID128612

反应详情

EQUATION

反应方程式

HRID 128612 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureunder reflux
  2. filtrationThe mixture was filtered
  3. distillationdistilled
  4. customThe fraction boiling at 167°-195° C. was collected
  5. custompurified by flash chromatography on silica