反应详情

温度

120 °C

To a solution of (2S)-2-(2-bromoisonicotinoylamino)-3-(3,4-dimethoxyphenyl)-1-propanol (1.2 g) in dimethylformamide (40 ml) are added potassium carbonate (0.88 g) and copper (I) iodide (0.61 g) at room temperature under nitrogen atmosphere. The mixture is heated with stirring at 120° C. for 30 minutes. To the reaction mixture is added 4-(3-pyridyl)phthalazin-1(2H)-one (1.42 g), and the mixture is heated with stirring at 130° C. for two hours. The reaction mixture is cooled to room temperature, and thereto is added aqueous ammonia. The mixture is extracted with chloroform, and the extract is washed, dried and concentrated. The residue is purified by silica gel chromatography (solvent; chloroform:acetone=1:1) to give (2S)-2-{2-[4-(3-pyridyl)phthalazin-1(2H)-on-2-yl]isonicotinoylamino}-3-(3,4-dimethoxyphenyl)-1-propanol (330 mg).

1. temperatureThe mixture is heated
2. temperaturethe mixture is heated
3. stirringwith stirring at 130° C. for two hours
4. temperatureThe reaction mixture is cooled to room temperature
5. extractionThe mixture is extracted with chloroform
6. washthe extract is washed
7. customdried
8. concentrationconcentrated
9. customThe residue is purified by silica gel chromatography (solvent; chloroform:acetone=1:1)