HRID1731927

反应详情

EQUATION

反应方程式

HRID 1731927 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture consisting of 20 g. (0.087 mole) of 2,6-dichloro-3-hydrazinoquinoxaline and 160 ml. (0.87 mole) of triethyl orthoacetate was heated with mechanical stirring under a dry nitrogen atmosphere in a preheated oil bath at 100° C. for a period of 20 hours to give a yellow suspension. The resulting mixture was cooled to room temperature and filtered, and the recovered solid product was subsequently washed with ethanol and air-dried to constant weight to ultimately afford 10.2 g. (46%) of pure 4,8-dichloro-1-methyl-[1,2,4]triazolo[4,3-a]quinoxaline, m.p. >280 ° C. Mass Spectrum: m/e, 254/252 (P+).

WORKUP

后处理

  1. customto give a yellow suspension
  2. temperatureThe resulting mixture was cooled to room temperature
  3. filtrationfiltered
  4. washthe recovered solid product was subsequently washed with ethanol
  5. customair-dried to constant weight to ultimately afford 10.2 g