HRID570004

反应详情

EQUATION

反应方程式

HRID 570004 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Mixed were 26.8 g of 1-amidino-4-benzylpiperazine sulfate and 133 ml of a 3% ethanol solution of sodium hydroxide, followed by an addition of 17.0 g of ethyl 2-cyano-3-ethoxyacrylate. After being refluxed for 5 hours, the reaction mixture was allowed to cool down. After distilling off ethanol from the reaction mixture, the residue was added with water and ethyl acetate. The resultant mixture was shaken. Precipitated colorless crystals of 2-(4-benzylpiperazino)-5-cyano-4-hydroxypyrimidine were collected by filtration, washed with water and then dried, thereby obtaining 7.4 g of 2-(4-benzylpiperazino)-5-cyano-4-hydroxypyrimidine (yield: 25%).

WORKUP

后处理

  1. additionMixed
  2. temperatureAfter being refluxed for 5 hours
  3. temperatureto cool down
  4. distillationAfter distilling off ethanol from the reaction mixture
  5. additionthe residue was added with water and ethyl acetate
  6. customPrecipitated colorless crystals of 2-(4-benzylpiperazino)-5-cyano-4-hydroxypyrimidine
  7. filtrationwere collected by filtration
  8. washwashed with water
  9. customdried