HRID979044

反应详情

EQUATION

反应方程式

HRID 979044 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into 40 ml of dichloromethane, was dissolved 6.5 g of 1-phenylpiperazine. To the solution, while being stirred and cooled in ice, was added dropwise 3.0 g of 2,4-dimethylallophanoyl chloride. After 0.5 hour of reaction at room temperature, the reaction mixture was washed with water and dried over anhydrous sodium sulfate. The solvent was removed by distillation and the residue was recrystallized from a mixture of ethanol and petroleum ether to obtain 4.0 g (72% yield) of 1-(2,4-dimethyl-allophanoyl)-4-phenylpiperazine having a melting point of 79°-80° C.

WORKUP

后处理

  1. temperaturecooled in ice
  2. customAfter 0.5 hour of reaction at room temperature
  3. washthe reaction mixture was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customThe solvent was removed by distillation
  6. customthe residue was recrystallized from a mixture of ethanol and petroleum ether