HRID1588025

反应详情

EQUATION

反应方程式

HRID 1588025 的结构方程式

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

Nitrobenzonitrile (5 g) was dissolved in 50 ml of dry N,N-dimethylformamide and mixed with 10.97 g of sodium azide and 9.03 g ammonium chloride. The resulting suspension was heated to 110° C. for 18 hours. The reaction mixture was concentrated in vacuo and the residue was dissolved in water (50 ml). The aqueous solution was washed with ethyl acetate and acidified with 1 N HCl solution. The aqueous phase was then extracted with ethyl acetate and the organic extracts were dried (sodium sulfate) and concentrated to give 8.5 g of the title compound as a white solid.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. dissolutionthe residue was dissolved in water (50 ml)
  3. washThe aqueous solution was washed with ethyl acetate
  4. extractionThe aqueous phase was then extracted with ethyl acetate
  5. dry with materialthe organic extracts were dried (sodium sulfate)
  6. concentrationconcentrated