HRID1729236

反应详情

EQUATION

反应方程式

HRID 1729236 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of sodium (1.84 g, 80 mmol) in ethanol (200 ml) was added phenylacetamidine hydrochloride (16.2 g, 95.0 mmol) and ethyl 4-phenylacetoacetate (15 g, 72.9 mmol). The mixture was heated under reflux with stirring for 5 days followed by cooling and evaporation in vacuo. Water (150 ml) was added to the residue causing a solid to precipitate which was filtered off and washed thoroughly with water and diethyl ether. Recrystallisation of the solid from a chloroform/hexane mixture afforded 6.9 g 2,4-di(phenylmethyl)-6-hydroxypyrimidine as a white solid. m.pt., 158°-160° C., M+ found: 276.

WORKUP

后处理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux
  3. temperatureby cooling
  4. customevaporation in vacuo
  5. additionWater (150 ml) was added to the residue
  6. customto precipitate which
  7. filtrationwas filtered off
  8. washwashed thoroughly with water and diethyl ether
  9. customRecrystallisation of the solid from a chloroform/hexane mixture