HRID2289552

反应详情

EQUATION

反应方程式

HRID 2289552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4,6-dichloropyrimidine (10.05 g), tert-butoxycarbonylpiperazine (11.94 g) and triethylamine (28.20 ml) in ethanol (150 ml) was heated at reflux for 18 hours. Solvent was evaporated and the residue dissolved in ethyl acetate and washed with water, saturated aqueous ammonium chloride solution, dried (Na2SO4) and evaporated. Recrystallisation from ethyl acetate/hexane gave, as a solid 1-(tert-butoxycarbonyl)-4-(6-chloro-pyrimidin-4-yl)piperazine (16.80 g).

WORKUP

后处理

  1. temperatureat reflux for 18 hours
  2. customSolvent was evaporated
  3. dissolutionthe residue dissolved in ethyl acetate
  4. washwashed with water, saturated aqueous ammonium chloride solution
  5. dry with materialdried (Na2SO4)
  6. customevaporated
  7. customRecrystallisation from ethyl acetate/hexane