反应详情

To a solution of 4-methoxy-3-(4-(morpholin-4-yl)phenyl)-1H-pyrazolo[4,3-c]pyridine (500 mg) obtained in Step G of Example 305 in anhydrous DMF (5 mL) was added sodium hydride (60% dispersion in mineral oil, 72.0 mg), and the mixture was stirred for 30 min. To the reaction mixture was added 7-oxabicyclo[4.1.0]heptane (1.60 g) at room temperature, and the mixture was stirred at 80° C. for 5 hr. The reaction mixture was added to ice-water, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel chromatography (ethyl acetate/petroleum ether) to give the title compound (400 mg).

1. stirringthe mixture was stirred at 80° C. for 5 hr
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer was washed with saturated brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationconcentrated under reduced pressure
6. customThe residue was purified by silica gel chromatography (ethyl acetate/petroleum ether)