HRID277038
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 solution of 0.20 g (0.0007 mol) 2-phenyl-7-pyridin-4-yl-[1,2,4]triazolo[1,5-a]pyridin-5-ylamine in 17.5 ml dimethylsulfoxide was treated with 0.69 g (0.001 mol) potassiumhydroxide(85%) for 20 minutes at room temperature. Then 0.10 g(0.0007 mol) 4-bromo-1-butene were added and stirring was continued for 40 hours. Saturated aqueous sodiumbicarbonate was added and the mixture was extracted with ethylacetate. Evaporation of the solvent and chromatography on silicagel with dichloromethane/methanol 97/3 gave 0.04 g(17%) but-3-enyl-(2-phenyl-7-pyridin-4-yl-[1,2,4]triazolo[1,5-a]pyridin-5-yl)-amine as beige crystals. MS m/e (%): 341 (M+, 21), 300 (100), 287 (65).
WORKUP
后处理
- extractionthe mixture was extracted with ethylacetate
- customEvaporation of the solvent and chromatography on silicagel with dichloromethane/methanol 97/3