反应详情

温度

60 °C

To a 25 mL round bottom flask with a stir bar was added 6-((3R,4R)-3-aminotetrahydro-2H-pyran-4-ylamino)-2-(2,4-dimethoxybenzyl)-7-fluoro-4-(pyrazolo[1,5-a]pyridin-3-yl)-1H-pyrrolo[3,4-c]pyridin-3(2H)-one (85 mg, 0.160 mmol) in TFA (5 mL). The mixture was heated at 60° C. for 1.5 h and then cooled to RT. The mixture was concentrated and purified via preparative HPLC to give a TFA salt of the title compound as a white solid (27 mg, 44.2%). 1H NMR (400 MHz, DMSO-d6) δ ppm 1.83-1.85 (m, 1H), 2.12-2.14 (m, 1H), 3.65-3.73 (m, 2H), 3.81-3.82 (m, 1H), 3.93-3.95 (m, 1H), 4.01-4.03 (m, 1H), 4.43 (s, 2H), 4.53-4.55 (m, 1H), 7.04 (t, J=6.83 Hz, 1H), 7.13 (d, J=4.88 Hz, 1H), 7.49 (t, J=8.05 Hz, 1H), 7.94 (br s, 1H), 8.36-8.42 (m, 2H), 8.78 (d, J=6.83 Hz, 1H), 9.33 (s, 1H). [M+H] calc'd for C19H19FN6O2, 383. found, 383.

1. temperaturecooled to RT
2. concentrationThe mixture was concentrated
3. custompurified via preparative HPLC