HRID277033

反应详情

EQUATION

反应方程式

HRID 277033 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a boiling suspension of 78.8 g(0.70 mol) potassium tert-butoxide in 400 ml tetrahydrofuran was slowly added over a period of 5 hours a mixture of 70.1 g (0.23 mol) 3-benzenesulfonylmethyl-5-phenyl-1H-[1,2,4]triazole and 30.5 g (0.23 mol) 3-(4-pyridinyl)-2-propenenitrile in 800 ml tetrahydrofuran. Boiling was continued for 18 hours and then the mixture was cooled to room temperature. Evaporation of the solvent and chromatography on silicael with dichloromethane/methanol 95/5 gave 19.8 g (29%) 2-phenyl-7-pyridin-4-yl-[1,2,4]triazolo[1,5-a]pyridin-5-ylamine as yellow crystals with mp. 207-210° C., MS m/e (%):287 (M+, 100).

WORKUP

后处理

  1. additionwas slowly added over a period of 5 hours
  2. customEvaporation of the solvent and chromatography on silicael with dichloromethane/methanol 95/5