HRID255728
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas gently refluxed for 72 hours
- washThe separated organic layer was washed with saturated aqueous sodium chloride solution
- dry with materialdried over magnesium sulfate
- customevaporated in vacuo
- customThe residual substance was recrystallized from diethyl ether-n-hexane