HRID462426

反应详情

EQUATION

反应方程式

HRID 462426 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 4,4'-dichlorobutyrophenone (4.5 g, 20.7 mmole) in 25 ml of acetone was added to a warm suspension of 2-chloro-4-(1-piperazinyl)benzenemethanol (4.7 g, 20.7 mole) in 50 ml acetone and 2.5 ml of triethylamine. The reaction mixture was refluxed for four days, cooled at -10° for three hours, and then filtered. The product was washed with a little acetone, triturated on the filter with water (four times, 50 ml), and air dried. Recrystallization from acetonitrile (65 ml) gave 3.0 g (35%), mp 137°-139°.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed for four days
  2. temperaturecooled at -10° for three hours
  3. filtrationfiltered
  4. washThe product was washed with a little acetone
  5. customtriturated on the
  6. filtrationfilter with water (four times, 50 ml), and air
  7. customdried
  8. customRecrystallization from acetonitrile (65 ml)
  9. customgave 3.0 g (35%), mp 137°-139°