HRID64588

反应详情

EQUATION

反应方程式

HRID 64588 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A mixture of 2-(p-bromophenyl)-5'-pentyl-5,2'-bipyrimidinyl (5.0 g, 0.013 mol), N-methyl-2-pyrrolidone (100 mL) and cuprous cyanide (1.16 g, 0.013 mol) was heated under reflux for 5 hours, followed by cooling the reaction mixture down to 40° C., adding toluene (500 ml) and 28% aqueous ammonia (100 ml), separating the resulting layers, washing the toluene layer with water till the washing water became neutral, drying the toluene layer over anhydrous sodium sulfate, distilling off toluene, and three times recrystallizing the residual solids from toluene to obtain 2-(p-cyanophenyl)-5'-pentyl-5,2'-bipyrimidinyl (2.1 g, 0.006 mol).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 5 hours
  3. customseparating the resulting layers
  4. washwashing the toluene layer with water till the washing water
  5. dry with materialdrying the toluene layer over anhydrous sodium sulfate
  6. distillationdistilling off toluene, and three times
  7. customrecrystallizing the residual solids from toluene