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 solution of 4-(3-pyridyl)phthalazin-1(2H)-one (167 mg) in dimethylformamide (5 ml) are added successively potassium carbonate (103 mg), copper iodide (70 mg) and 2-bromo-4-[6,7-dimethoxy-2-(4-pyridyl)methyl-phthalazin-1(2H)-on-4-yl]pyridine (335 mg) under nitrogen atmosphere, and the mixture is refluxed for two hours. The reaction mixture is cooled, and thereto is added aqueous ammonia. The mixture is extracted with chloroform, and the extract is washed, dried, concentrated, and purified by silica gel column chromatography (solvent; chloroform:methanol=19:1) to give 4-[6,7-dimethoxy-2-(4-pyridyl)methylphthalazin-1(2H)-on-4-yl]-2-[4-(3-pyridyl)-phthalazin-1(2H)-on-2-yl]pyridine (216 mg).
WORKUP
后处理
- temperaturethe mixture is refluxed for two hours
- temperatureThe reaction mixture is cooled
- extractionThe mixture is extracted with chloroform
- washthe extract is washed
- customdried
- concentrationconcentrated
- custompurified by silica gel column chromatography (solvent; chloroform:methanol=19:1)