HRID2051622

反应详情

EQUATION

反应方程式

HRID 2051622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

To a mixture of 68.5 g. of p-chlorobenzonitrile and 24.0 g. of sodium hydride (50% in mineral oil) in 250 ml. of ether is added, 26.1 ml. of acetonitrile and 2 ml. of isopropanol. The mixture is stirred and refluxed on a steam bath for 6 hours and then stirred overnight at room temperature. A 5 ml. portion of methanol and 250 ml. of water are added. The ether is boiled away on a steam bath and the mixture is filtered. The solid is dissolved in warm ethyl acetate and filtered. The filtrate is evaporated to a solid giving β-amino-4-chlorocinnamonitrile.

WORKUP

后处理

  1. additionTo a mixture of 68.5 g
  2. temperaturerefluxed on a steam bath for 6 hours
  3. stirringstirred overnight at room temperature
  4. filtrationthe mixture is filtered
  5. dissolutionThe solid is dissolved in warm ethyl acetate
  6. filtrationfiltered
  7. customThe filtrate is evaporated to a solid