HRID1361013

反应详情

EQUATION

反应方程式

HRID 1361013 的结构方程式

CONDITIONS

反应条件

温度
125 °C

PROCEDURE

实验过程

The above naphthoic acid amide (10 g, 37 mmol) was dissolved in N,N-dimethylformamide (200 mL) and sodium azide (2.63 g, 40 mmol) and ammonium chloride (2.16 g, 40 mmol) were added and the mixture heated at 125° C. for 6 hours. Sodium azide (1.2 g) and ammonium chloride (0.98 g) were added and the mixture heated at 125° C. for 16 hours. After cooling, the mixture was poured into water (1.5 l) and stirred at room temperature for 30 minutes. The solid formed was filtered off, washed with water and dried in vacuo at 50° C. for 3 days affording 9.69 g (84%) of the title compound as a solid which could be further purified by treatment with ethanol at reflux temperature.

WORKUP

后处理

  1. temperaturethe mixture heated at 125° C. for 16 hours
  2. temperatureAfter cooling
  3. customThe solid formed
  4. filtrationwas filtered off
  5. washwashed with water
  6. customdried in vacuo at 50° C. for 3 days