HRID2289552
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureat reflux for 18 hours
- customSolvent was evaporated
- dissolutionthe residue dissolved in ethyl acetate
- washwashed with water, saturated aqueous ammonium chloride solution
- dry with materialdried (Na2SO4)
- customevaporated
- customRecrystallisation from ethyl acetate/hexane