HRID2255376
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionTo a dry flask under a nitrogen atmosphere was added 0.9 g
- temperatureThe mixture was slowly heated
- temperatureto reflux
- temperaturewas cooled
- customto precipitate the crude product
- filtrationThe crystals were filtered
- washwashed of residual thionyl chloride
- customto obtain 1.0 g