反应详情

温度

25 °C

To a 50 mL round-bottomed flask was added N-(6-(6-chloro-5-(methylsulfonamido)pyridin-3-yl)imidazo[1,2-b]pyridazin-2-yl)acetamide (Example 19) (0.404 g, 1.06 mmol), chloroform (20 mL) and N-iodosuccinimide (0.48 g, 2.1 mmol). The mixture was stirred at 25° C. for 1 h then poured into CH2Cl2 (200 mL) and water (200 mL). The solution contained a precipitate. This was filtered and the filtercake was washed with water and then dried under vacuum. The solid was taken up in MeOH/CH2Cl2 and concentrated onto Celite® (diatomaceous earth). Purification by silica gel chromatography (2.0 to 10% MeOH/CH2Cl2) afforded the title compound as a yellow solid (0.199 g, 37%). MS (ESI, positive ion) m/z: 506.4 (M+1). 1H NMR (400 MHz, DMSO-d6) δ ppm 2.07 (s, 3H), 3.20 (s, 3H), 7.96 (d, J=9.6 Hz, 1H), 8.20 (d, J=9.4 Hz, 1H), 8.55 (d, J=2.2 Hz, 1H), 8.98 (d, J=2.2 Hz, 1H), 9.98 (s, 1H), 10.13 (s, 1H).

1. filtrationThis was filtered
2. washthe filtercake was washed with water
3. customdried under vacuum
4. concentrationconcentrated onto Celite® (diatomaceous earth)
5. customPurification by silica gel chromatography (2.0 to 10% MeOH/CH2Cl2)