HRID2255376

反应详情

EQUATION

反应方程式

HRID 2255376 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a dry flask under a nitrogen atmosphere was added 0.9 g. (4.8 mmoles) of 4-(4-hydroxybutyl)-2,6-dimethylmorpholine in 2.5 ml. of chloroform. The solution was stirred and heated to 40° C. and 0.49 ml. (6.72 mmoles) of thionyl chloride in 2.5 ml. of chloroform was added slowly. The mixture was slowly heated to reflux and held for two hours, then was cooled and diluted with diethyl ether to precipitate the crude product. The crystals were filtered and washed of residual thionyl chloride using diethyl ether to obtain 1.0 g. (85% yield) of 4-(4-chlorobutyl)-2,6-dimethylmorpholine hydrochloride.

WORKUP

后处理

  1. additionTo a dry flask under a nitrogen atmosphere was added 0.9 g
  2. temperatureThe mixture was slowly heated
  3. temperatureto reflux
  4. temperaturewas cooled
  5. customto precipitate the crude product
  6. filtrationThe crystals were filtered
  7. washwashed of residual thionyl chloride
  8. customto obtain 1.0 g