反应详情

To a suspension of (6-chloro-imidazo[1,2-b]pyridazin-3-yl)-(7-fluoro-quinolin-6-yl)-methanol (1.8 g, 5.48 mmol) in acetone (200 mL) was added 2-iodoxybenzoic acid (8.52 g, 45%, 13.69 mmol) and the reaction mixture was stirred at reflux for 1 day. The solvent was removed under reduced pressure and the residue was dissolved in 200 mL of water. The solution was basified by 3N NaOH solution and the precipitate was collected, washed with water and dried over vacuum oven to afford 1.7 g (yield: 95%) title compound as a gray solid. 1H-NMR (400 MHz, DMSO-d6) δ ppm 9.04 (dd, 1H), 8.56 (d, 1H), 8.47 (m, 2H), 8.41 (s, 1H), 7.92 (d, 1H), 7.75 (d, 1H), 7.64 (q, 1H). LCMS (method B): [MH]+=327, tR=2.03 min.

1. temperatureat reflux for 1 day
2. customThe solvent was removed under reduced pressure
3. dissolutionthe residue was dissolved in 200 mL of water
4. customthe precipitate was collected
5. washwashed with water
6. customdried over vacuum oven