反应详情

Under an argon atmosphere, to a solution of 5-methoxy-3-(1-phenyl-1H-pyrazol-5-yl)pyridazin-4-ol (2.0 g) in dimethylformamide (40 mL) was added 60% sodium hydride (596 mg) with stirring under ice-cooling, and the mixture was stirred at the same temperature for 1.5 hr. Then, (bromomethyl)cyclopropane (1.085 mL) was added, and the mixture was stirred at room temperature for 16 hr. To the reaction mixture was added methanol, and the mixture was concentrated under reduced pressure to dryness. The residue was purified by silica gel column chromatography (ethyl acetate/methanol) and crystallized from methanol/ethyl acetate to give the title compound (2.12 g) as white prisms.

1. temperaturecooling
2. stirringthe mixture was stirred at the same temperature for 1.5 hr
3. stirringthe mixture was stirred at room temperature for 16 hr
4. concentrationthe mixture was concentrated under reduced pressure to dryness
5. customThe residue was purified by silica gel column chromatography (ethyl acetate/methanol)
6. customcrystallized from methanol/ethyl acetate