HRID1444849

反应详情

EQUATION

反应方程式

HRID 1444849 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 4-bromo-3-fluorophenylcyclopropanenitrile (21 mmoles) in methanol (10 ml) is added with a 35% NaOH aqueous solution (40 ml) and a 35% H2O2 aqueous solution (3 ml), then is refluxed for 4 hours, cooled at room temperature and added with 2N HCl (250 ml). The precipitated solid is collected by filtration and redissolved in a 5% NaHCO3 aqueous solution (300 ml). The insoluble fraction is filtered off and the clear filtrate is acidified to pH=2 with 2N HCl. The product precipitates as a white solid, which is recovered by filtration and dried under vacuum.

WORKUP

后处理

  1. filtrationThe precipitated solid is collected by filtration
  2. dissolutionredissolved in a 5% NaHCO3 aqueous solution (300 ml)
  3. filtrationThe insoluble fraction is filtered off
  4. customThe product precipitates as a white solid, which
  5. filtrationis recovered by filtration
  6. customdried under vacuum