HRID266871

反应详情

EQUATION

反应方程式

HRID 266871 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(Dimethylamino)butanol (88.5g) was added dropwise at 0° C. over 2 hours to stirred thionyl chloride (93.4 g) then the mixture was stirred at ambient temperature for 1 hour and poured into ethanol (500 ml). The stirred solution was heated under reflux for 10 minutes, then the solvent was removed in vacuo. The solid residue crystallised from ethanol as a white solid which was collected by filtration, washed with ethanol, and dried in vacuo at ambient temperature for 24 hours to give 1-chloro-4-(dimethylamino)butane hydrochloride as a white solid (115 g), m.p. 100°-105° C.

WORKUP

后处理

  1. temperatureThe stirred solution was heated
  2. temperatureunder reflux for 10 minutes
  3. customthe solvent was removed in vacuo
  4. customThe solid residue crystallised from ethanol as a white solid which
  5. filtrationwas collected by filtration
  6. washwashed with ethanol
  7. customdried in vacuo at ambient temperature for 24 hours