HRID1172680

反应详情

EQUATION

反应方程式

HRID 1172680 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

4.0 g 1-Bromo-4-fluoro-2-vinyl-benzene and 1.87 g copper (I) cyanide were dissolved in 16 ml dimethylformamide and heated under microwave irradiation at 200° C. for 25 minutes. The cooled reaction mixture was poured into 200 ml 1 M HCl and extracted five times with portions of 60 ml ethyl acetate. The combined organic layers were washed with 100 ml 1 N HCl, dried over MgSO4, then the solvent was removed in vacuo and the resulting residue purified on silica gel with the eluent heptane=>n-heptane:ethyl acetate=6:1 to obtain 1.77 g 4-Fluoro-2-vinyl-benzonitrile as a solid.

WORKUP

后处理

  1. customThe cooled reaction mixture
  2. extractionextracted five times with portions of 60 ml ethyl acetate
  3. washThe combined organic layers were washed with 100 ml 1 N HCl
  4. dry with materialdried over MgSO4
  5. customthe solvent was removed in vacuo
  6. customthe resulting residue purified on silica gel with the eluent heptane=>n-heptane