HRID255728

反应详情

EQUATION

反应方程式

HRID 255728 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 5 -cyanomethyl-6-methyl-4-(3-nitrophenyl)-2-phenylpyrimidine (5 g), conc. sulfuric acid (12 g) and ethanol (50 ml) was gently refluxed for 72 hours. The reaction mixture was poured into a suspension of chloroform (200 ml) and water (100 ml), and then adjusted to pH 8.5 with 10% aqueous sodium carbonate solution. The separated organic layer was washed with saturated aqueous sodium chloride solution, dried over magnesium sulfate and evaporated in vacuo. The residual substance was recrystallized from diethyl ether-n-hexane to give ethyl 6-methyl-4-(3-nitrophenyl)-2-phenyl-5-pyrimidinylacetate (3.7 g).

WORKUP

后处理

  1. temperaturewas gently refluxed for 72 hours
  2. washThe separated organic layer was washed with saturated aqueous sodium chloride solution
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residual substance was recrystallized from diethyl ether-n-hexane