HRID1448434

反应详情

EQUATION

反应方程式

HRID 1448434 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

102.75 G. of 4-[5-(4-n-butylphenyl)-2-pyrimidyl] benzoic acid amide are refluxed for 80 minutes in a mixture of 1500 ml. of ethylene chloride and 34 ml. of phosphorus oxychloride with stirring. The mixture, diluted with ether, is washed with 2-N sodium hydroxide solution and then with water until neutral. After evaporation of the organic phase, which has been dried over sodium sulfate, there is obtained 5-(4-n-butylphenyl)-2-(4-cyanophenyl)pyrimidine which is filtered on a short silica gel column and subsequently recrystallized from methylene chloride/methanol; melting point 94.7° C.; clearing point 246°-246.7° C.

WORKUP

后处理

  1. washis washed with 2-N sodium hydroxide solution
  2. customAfter evaporation of the organic phase, which
  3. dry with materialhas been dried over sodium sulfate