HRID2403112

反应详情

EQUATION

反应方程式

HRID 2403112 的结构方程式

PROCEDURE

实验过程

A solution of 2-cyanophenylacetonitrile (1 g, 7 mmol) and hydroxylamine (1.7 cm3, 28.1 mmol, 4 eq) in EtOH (25 cm3) were stirred under reflux for 60 hours, after which the volatiles were removed under reduced pressure. The residue was recrystallised from EtOH-water (1:4, 15 cm3) to give the cyclised product 3-aminoisoquinolin-1(4H)-one oxime or 3-(hydroxyamino)-3,4-dihydroisoquinolin-1-amine (1.15 g, 85.9%) as a solid, mp 92.5-94.5° C.

WORKUP

后处理

  1. temperatureunder reflux for 60 hours
  2. customafter which the volatiles were removed under reduced pressure
  3. customThe residue was recrystallised from EtOH-water (1:4, 15 cm3)