反应详情

温度

65 °C

To a solution of (S)-6-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-fluoro-2-(1-(4-fluorophenyl)ethylamino)nicotinonitrile (Method 42; 0.5 g, 1.3 mmol) in MeOH (50 ml) was added KOH solution (25%, 2 ml), followed by addition of H2O2 (30%, 0.1 ml). The resulting dark red solution was heated to 65° C. for 1 hour, cooled, and concentrated. The resulting residue was dissolved in EtOAc (50 ml), washed with water (30 ml), dried, filtered, and concentrated. The resulting solid was purified by column chromatography (DCM:MeOH=30:1) to give the title compound (0.30 g, 60%). MS: Calcd.: 398. Found: [M+H]+ 399.

1. temperaturecooled
2. concentrationconcentrated
3. dissolutionThe resulting residue was dissolved in EtOAc (50 ml)
4. washwashed with water (30 ml)
5. customdried
6. filtrationfiltered
7. concentrationconcentrated
8. customThe resulting solid was purified by column chromatography (DCM:MeOH=30:1)