HRID1583413

反应详情

EQUATION

反应方程式

HRID 1583413 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 20.6 g of 5-pyrimidinehexanol in 80 ml of dichloromethane was cooled in an ice bath as a solution of 12.3 ml of thionyl chloride in 40 ml of dichloromethane was added dropwise. The mixture was stirred at room temperature for 1 hour and at reflux temperature for 1 hour, was concentrated, azeotroped with toluene, diluted with dichloromethane and washed with water, saturated sodium bicarbonate, and brine. Evaporation gave 22.3 g of 6-(5-pyrimidinyl)hexylchloride.

WORKUP

后处理

  1. additionwas added dropwise
  2. temperatureat reflux temperature for 1 hour
  3. concentrationwas concentrated
  4. customazeotroped with toluene
  5. additiondiluted with dichloromethane
  6. washwashed with water, saturated sodium bicarbonate, and brine
  7. customEvaporation