HRID46558

反应详情

EQUATION

反应方程式

HRID 46558 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A 150 ml. portion of ammonia is condensed in a reaction flash and a small piece of sodium is added. The blue color is discharged by the addition of ferric chloride and 3.22 g. of sodium are added. After the cooler is discharged 5.75 ml. of acetonitrile in 10 ml. of ether are added. The reaction is cooled in a dry ice-acetone bath and 13.3 g. of 2-chlorobenzonitrile in 25 ml. of tetrahydrofuran are added dropwise. The ammonia is allowed to evaporate, the solvent is blown off with nitrogen and water is added. The mixture is extracted with methylene chloride. The organic extracts are dried over sodium sulfate and filtrate through magnesol. The filtrate is evaporated with the addition of hexanes giving β-amino-2-chlorocinnamonitrile as a white crystalline solid.

WORKUP

后处理

  1. customcondensed
  2. customin a reaction flash
  3. temperatureThe reaction is cooled in a dry ice-acetone bath
  4. customto evaporate
  5. additionis added
  6. extractionThe mixture is extracted with methylene chloride
  7. dry with materialThe organic extracts are dried over sodium sulfate and filtrate through magnesol
  8. customThe filtrate is evaporated with the addition of hexanes