HRID562452

反应详情

EQUATION

反应方程式

HRID 562452 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

At RT, 4.4 ml (4.5 g, 89.7 mmol) of hydrazine hydrate are added dropwise with stirring to a solution of 1.9 g (7.5 mmol) of 4-chloro-6-(4-cyclobutylpiperazin-1-yl)pyrimidine in 28 ml of ethanol. The reaction solution is stirred at 80° C. for 16 h. For work-up, the mixture is concentrated under reduced pressure, the residue is triturated repeatedly with diethyl ether, and the precipitated solid is filtered off and dried under reduced pressure. The residue is then purified by column chromatography on silica gel (mobile phase dichloromethane/methanol 10/2). Yield: 1.5 g (80% of theory)

WORKUP

后处理

  1. concentrationFor work-up, the mixture is concentrated under reduced pressure
  2. customthe residue is triturated repeatedly with diethyl ether
  3. filtrationthe precipitated solid is filtered off
  4. customdried under reduced pressure
  5. customThe residue is then purified by column chromatography on silica gel (mobile phase dichloromethane/methanol 10/2)