反应详情

温度

83 °C

A mixture of (S)-6-(5-cyclopropyl-1H-pyrazol-3-ylamino)-5-fluoro-2-(1-(4-fluorophenyl)ethylamino)nicotinic acid (Method 40; 0.03 g, 0.08 mmol), triethylamine (0.02 g, 0.22 mmol), and DPPA (0.04 g, 0.15 mmol) in t-BuOH (2 ml) was heated to 83° C. for 5 hours. The reaction was cooled, concentrated, and then dissolved in DCM (30 ml). The organic layer was washed with water (50×2 ml), dried, filtered, and concentrated. The resulting solid was purified by column chromatography (DCM:MeOH=15:1) to give the title compounds (0.01 g, 30%). NMR (400 MHz, CD3OD) 7.48-7.44 (m, 2H), 7.24 (d, J=10.3 Hz, 1H), 7.06-7.02 (m, 2H), 5.93 (br s, 1H), 5.76-5.71 (m, 1H), 1.99 (d, J=7.2 Hz, 3H), 1.90-1.84 (m, 1H), 0.96-0.94 (m, 2H), 0.64-0.63 (m, 2H). MS: Calcd.: 396. Found: [M+H]+ 397.

1. temperatureThe reaction was cooled
2. concentrationconcentrated
3. dissolutiondissolved in DCM (30 ml)
4. washThe organic layer was washed with water (50×2 ml)
5. customdried
6. filtrationfiltered
7. concentrationconcentrated
8. customThe resulting solid was purified by column chromatography (DCM:MeOH=15:1)