HRID79274

反应详情

EQUATION

反应方程式

HRID 79274 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (2-methoxy-6-methylpyridin-3-yl)methanol (4.7 g, 30.7 mmol) in dichloromethane (150 mL) was added triphenylphosphine (12.1 g, 46.0 mmol). The mixture was cooled in an ice bath with stirring under an atmosphere of nitrogen. Carbon tetrabromide (15.3 g; 46.0 mmol) was added and the mixture was stirred for 90 minutes. The mixture was concentrated under reduced pressure and purified using column chromatography on silica, eluting with dichloromethane/hexanes (1:1) to give 3-(bromomethyl)-2-methoxy-6-methylpyridine (2.0 g).

WORKUP

后处理

  1. temperatureThe mixture was cooled in an ice bath
  2. stirringthe mixture was stirred for 90 minutes
  3. concentrationThe mixture was concentrated under reduced pressure
  4. custompurified
  5. washeluting with dichloromethane/hexanes (1:1)