反应详情

温度

0 °C

A solution of 4-(4-(1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazole-4-carboxamido)-3-fluorophenoxy)picolinamide (370 mg (a little wet), 0.746 mmol) in EtOAc (4.5 mL), CH3CN (4.5 mL) and H2O (2.5 mL) was cooled and stirred at 0° C. for 30 minutes and then PhI(OAc)2 (288 mg, 0.895 mmol) was added. The resulted mixture was stirred at 0° C. for another 30 minutes, then warmed up to rt and stirred for 7 hours. The mixture was filtered and the filter cake was washed with EtOAc (5 mL). The filtrate was concentrated in vacuo and the residue was purified by a silica column gel chromatography (CH2Cl2/MeOH (v/v)=250/9), followed by purifying again by silica gel column chromatography (CH2Cl2/MeOH (v/v)=50/1) to give the title compound as a beige white solid (46 mg, 17.3%).

1. stirringThe resulted mixture was stirred at 0° C. for another 30 minutes
2. temperaturewarmed up to rt
3. stirringstirred for 7 hours
4. filtrationThe mixture was filtered
5. washthe filter cake was washed with EtOAc (5 mL)
6. concentrationThe filtrate was concentrated in vacuo
7. customthe residue was purified by a silica column gel chromatography (CH2Cl2/MeOH (v/v)=250/9)
8. customby purifying again by silica gel column chromatography (CH2Cl2/MeOH (v/v)=50/1)