HRID1390620

反应详情

EQUATION

反应方程式

HRID 1390620 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3,5-dichloro-4-methoxyaniline (16.0g) and bis-(2-chloroethyl)amine hydrochloride (14.77g) in n-butanol (100 ml) was stirred under reflux for 48 hr. Anhydrous potassium carbonate (11.45g) was added and the resulting mixture was stirred under reflux for a further 24 hr., then filtered hot. The solid which precipitated on cooling was crystallised from ethanol-ether to give 1-(3,5-dichloro-4-methoxyphenyl)piperazine hydrochloride (3.7g) m.p. 252°-255°.

WORKUP

后处理

  1. temperatureunder reflux for 48 hr
  2. stirringthe resulting mixture was stirred
  3. temperatureunder reflux for a further 24 hr
  4. filtration, then filtered hot
  5. customThe solid which precipitated
  6. temperatureon cooling
  7. customwas crystallised from ethanol-ether