HRID1739415

反应详情

EQUATION

反应方程式

HRID 1739415 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. temperaturethe mixture is refluxed for two hours
  2. temperatureThe reaction mixture is cooled
  3. extractionThe mixture is extracted with chloroform
  4. washthe extract is washed
  5. customdried
  6. concentrationconcentrated
  7. custompurified by silica gel column chromatography (solvent; chloroform:methanol=19:1)