HRID1389278

反应详情

EQUATION

反应方程式

HRID 1389278 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture of 80 g 1-(ethoxycarbonyl)piperazine and 41 g of 2-(4-fluorophenyl)ethyl bromide is kept at room temperature overnight and then heated to 100° C. for 1 hour. After cooling, it is diluted with 50 ml water and extracted with benzene. The extract is washed with water and then shaken with 5% hydrochloric acid. The separated solid hydrochloride is filtered off, washed with a small quantity of water, decomposed by treatment with aqueous ammonia and the base isolated again by extraction with benzene. Processing of the extract affords 51 g (91%) of the crude 1-(ethoxycarbonyl)-4-(2-[4-fluorophenyl]ethyl)piperazine, b.p. 198° C./3 Torr.

WORKUP

后处理

  1. temperatureAfter cooling
  2. extractionextracted with benzene
  3. washThe extract is washed with water
  4. filtrationThe separated solid hydrochloride is filtered off
  5. washwashed with a small quantity of water
  6. customthe base isolated again by extraction with benzene