HRID396149

反应详情

EQUATION

反应方程式

HRID 396149 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 6-phenyl-[1,2,4]triazine-4-oxide (27 g, 156 mmol) and triethyl phosphite (500 ml) was heated under reflux for 30 min. The cooled reaction mixture was evaporated tit vacuo and the residue was purified by flash chromatography (SiO2; 50% Et2O in hexanes) to afford 19 g (121 mmol, 78%) of 6-phenyl-[1,2,4]triazine as a yellow solid. δH (400 MHz; CDCl3) 7.56-7.59 (3H, m, aromatics), 8.10-8.14 (2H, m, aromatics), 9.03 (1H, s, triazine H5), 9.65 (1H, s, triazine H3); m/z (ES+) 158 (M++H, 100%).

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 30 min
  3. customThe cooled reaction mixture
  4. customwas evaporated tit vacuo
  5. customthe residue was purified by flash chromatography (SiO2; 50% Et2O in hexanes)