HRID2289561

反应详情

EQUATION

反应方程式

HRID 2289561 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 (3.60 g), 1-(tert-butoxycarbonyl)-4-(-4-piperidylcarbonyl)piperazine (6.00 g) and sodium hydrogen carbonate (4.20 g) in ethanol (100 ml) was heated at reflux for 6 hours. Solvent was evaporated and the residue dissolved in ethyl acetate and washed with water, dried (Na2SO4) and evaporated. The residue was recrystallised from ethyl acetate to give, as a solid 1-(tert-butoxycarbonyl)-4-[1-(6-chloro-pyrimidin-4-yl)-piperidin-4-ylcarbonyl]piperazine (7.40 g).

WORKUP

后处理

  1. temperatureat reflux for 6 hours
  2. customSolvent was evaporated
  3. dissolutionthe residue dissolved in ethyl acetate
  4. washwashed with water
  5. dry with materialdried (Na2SO4)
  6. customevaporated
  7. customThe residue was recrystallised from ethyl acetate