HRID12269

反应详情

EQUATION

反应方程式

HRID 12269 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
130 °C

PROCEDURE

实验过程

A mixture of 2 g of diethyl 2-[2-(2-ethylaminopyrimidin-4-yl)-2-oxo-ethyl]-2-hydroxy-malonate, 485 mg of hydrazine hydrochloride and 20 ml of ethanol is stirred under reflux for 24 hours. After cooling while stirring, the precipitate is filtered off with suction, heated in 4 ml of N-methylpyrrolidinone (NMP) at 130° C. for 3 hours and, after cooling, mixed with 15 ml of n-heptane and stirred. The precipitate is then filtered off with suction and stirred with methylene chloride, again filtered off with suction and dried.

WORKUP

后处理

  1. temperatureunder reflux for 24 hours
  2. temperatureAfter cooling
  3. stirringwhile stirring
  4. filtrationthe precipitate is filtered off with suction
  5. temperatureafter cooling
  6. additionmixed with 15 ml of n-heptane
  7. stirringstirred
  8. filtrationThe precipitate is then filtered off with suction
  9. stirringstirred with methylene chloride
  10. filtrationagain filtered off with suction
  11. customdried