HRID267730

反应详情

EQUATION

反应方程式

HRID 267730 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a solution of 8.2 g of 1-(2-pyrimidinyl)-piperazine and 5g of anhydrous triethylamine in 200 ml of anhydrous tetrahydrofuran, there were added dropwise a solution of 9.1 g of 5-coumaranyl carboxylic acid chloride in 20 ml of tetrahydrofuran. After the completion of the addition, the reaction mixture was heated at 60° C for 2 hours, then the so-formed precipitate was suction-filtered off. The filtrate was evaporated under reduced pressure and the crystalline residue was washed with water then recrystallized in 70 ml of ethanol. There were obtained 12 g of 1-(5-coumaranyl carbonyl)-4-(2-pyrimidinyl) piperazine, melting (K) at 149°-150° C.

WORKUP

后处理

  1. additionAfter the completion of the addition
  2. filtrationthe so-formed precipitate was suction-filtered off
  3. customThe filtrate was evaporated under reduced pressure
  4. washthe crystalline residue was washed with water
  5. customthen recrystallized in 70 ml of ethanol