HRID396149
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureunder reflux for 30 min
- customThe cooled reaction mixture
- customwas evaporated tit vacuo
- customthe residue was purified by flash chromatography (SiO2; 50% Et2O in hexanes)