HRID485384
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
PROCEDURE
实验过程
A solution of 4-[3-[(dimethylamino)methyl]phenoxy]butanal (0.5 g) and 3-phenyl methyl-1H-1,2,4-triazole-5-amine (0.39 g) in dry toluene (60 ml) was heated under reflux during 3 h. The solvent was evaporated and replaced with methanol (50 ml). Sodium borohydride (0.4 g) was added and the mixture was stirred at 20° during 2 h. The methanol was evaporated and the residue partitioned between water and ethyl acetate. The organic extract was evaporated and the residue was purified by column chromatography to give the title compound, which crystallised from a mixture of ethyl acetate and cyclohexane as pale yellow crystals (0.09 g) m.p. 131°-3°; tlc system A,Rf 0.6.
WORKUP
后处理
- temperatureunder reflux during 3 h
- customThe solvent was evaporated
- additionSodium borohydride (0.4 g) was added
- customThe methanol was evaporated
- customthe residue partitioned between water and ethyl acetate
- extractionThe organic extract
- customwas evaporated
- customthe residue was purified by column chromatography