HRID277011
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
To a boiling suspension of 5.9 g(0.12 mol) sodiumhydride (55%) in 100 ml tetrahydrofuran was slowly added over a period of 6 hours a mixture of 10.1 g (0.035 mol) 3-benzenesulfonyl-methyl-5-furan-2-yl-1H-[1,2,4]triazole and 4.56 g (0.035 mol) 3-(4-pyridinyl)-2-propenenitrile in 400 ml tetrahydrofuran. Boiling was continued for 15 hours and then 50 ml methanol were added at room temperature. Evaporation of the solvent and chromatography on silicagel with dichloromethane/methanol 95/5 gave 1.3 g (13%) 2-furan-2-yl-7-pyridin-4-yl-[1,2,4]triazolo [1,5-a]pyridin-5-ylamine as yellow crystals with mp. 294-296° C.
WORKUP
后处理
- additionwas slowly added over a period of 6 hours
- customEvaporation of the solvent and chromatography on silicagel with dichloromethane/methanol 95/5