HRID1789058

反应详情

EQUATION

反应方程式

HRID 1789058 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

36 ml of thionyl chloride are added dropwise to a cooled suspension of 57 g of (±)-1-[4-methoxy-2-pyridyl]ethanol in 400 ml of dichloromethane, in such a way that the internal temperature does not exceed 15° C. The mixture is then heated under reflux for 2.5 h, treated with 300 ml of toluene and concentrated to 150 ml. The reaction product which has precipitated is filtered off with suction and rinsed with cold toluene and petroleum ether. This gives 76.4 g (98.2%) of the title compound of m.p. 113°-116° C.

WORKUP

后处理

  1. customdoes not exceed 15° C
  2. temperatureThe mixture is then heated
  3. temperatureunder reflux for 2.5 h
  4. concentrationconcentrated to 150 ml
  5. customThe reaction product which has precipitated
  6. filtrationis filtered off with suction
  7. washrinsed with cold toluene and petroleum ether