HRID1703790

反应详情

EQUATION

反应方程式

HRID 1703790 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred mixture of 8g of 1[1-(4'-chloro[1,1']biphenyl-4-yl)ethyl]piperazine, 2.7g of sodium bicarbonate in 75 ml of absolute ethanol, add in a dropwise fashion 5.25g of cinnamyl bromide. Reflux the reaction mixture for 6 hours, concentrate in vacuo, and treat with 50 ml of 10% hydrochloric acid solution. Filter the dihydrochloride and recrystallize from 80% ethanol, m.p. 273°-275°. The free base has a melting point of 108°-109° after recrystallization from acetonitrile.

WORKUP

后处理

  1. temperatureReflux the reaction mixture for 6 hours
  2. concentrationconcentrate in vacuo
  3. additiontreat with 50 ml of 10% hydrochloric acid solution
  4. filtrationFilter the dihydrochloride
  5. customrecrystallize from 80% ethanol, m.p. 273°-275°
  6. customafter recrystallization from acetonitrile