反应详情

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0 °C

To a suspension of N-(4-((2-aminopyridin-4-yl)oxy)phenyl)-1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamide (100 mg, 0.241 mmol) in THF/DMF (15 mL/1 mL) was added Et3N (0.06 mL, 0.482 mmol). The suspension was cooled to 0° C., then a solution of cyclobutanecarbonyl chloride (31.0 mg, 0.265 mmol) in THF (5 mL) was added to the reaction system drop wise over 1 hour. The reaction was stirred at rt for 5 hours, and then diluted with EtOAc (20 mL). The resulted mixture was washed with water (25 mL×3), followed by washing with brine (25 mL), dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The residue was purified by a silica gel column chromatography (DCM/EtOAc/MeOH (v/v)=100/25/1) to give the title compound as a white solid (30 mg, 25%).

1. washThe resulted mixture was washed with water (25 mL×3)
2. washby washing with brine (25 mL)
3. dry with materialdried over anhydrous Na2SO4
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe residue was purified by a silica gel column chromatography (DCM/EtOAc/MeOH (v/v)=100/25/1)