HRID1032699

反应详情

EQUATION

反应方程式

HRID 1032699 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Potassium hydroxide (3.1 g) was added to 200 ml of ethanol, and the mixture was stirred for 30 minutes. Then, 12.4 g of 1-amidino-4-benzylpiperazine sulfate was added. The mixture was stirred at room temperature for 10 minutes. To the solution was added 12.4 g of diethyl acetylsuccinate. The mixture was refluxed for 2 hours. Then, 200 ml of toluene was added, and the mixture was refluxed for 3 hours. After the reaction, ethanol was evaporated, and the residue was poured into 50 ml of an aqueous solution of hydrochloric acid. NaHCO3 was added to the solution to neutralize it. The precipitated solid was washed with water and dried over P2O5 to give 2.55 g (yield 15%) of 2-(4-benzylpiperazino)-5-ethoxycarbonylmethyl-4-hydroxy-6-methylpyrimidine as a white solid.

WORKUP

后处理

  1. stirringThe mixture was stirred at room temperature for 10 minutes
  2. temperatureThe mixture was refluxed for 2 hours
  3. temperaturethe mixture was refluxed for 3 hours
  4. customwas evaporated
  5. additionthe residue was poured into 50 ml of an aqueous solution of hydrochloric acid
  6. additionNaHCO3 was added to the solution
  7. washThe precipitated solid was washed with water
  8. dry with materialdried over P2O5