反应详情

To a solution of 6-(cis-2-amino-3,3-difluorocyclohexylamino)-2-(2,4-dimethoxybenzyl)-7-fluoro-4-(1-methyl-1H-pyrazol-4-yl)-1H-pyrrolo[3,4-c]pyridin-3(2H)-one (21 mg, 0.040 mmol) in DCM (300 μL) was added TFA (500 μL, 6.49 mmol). The reaction mixture was stirred at ambient temperature for 12 h then an additional 3 h at 50° C. The mixture was subsequently concentrated to a dark oil and diluted with DMF (1 mL) which was purified via preparative HPLC and lyophilized to give a TFA salt of the title compound as a fluffy white solid (3.6 mg, 19%). 1H NMR (400 MHz, DMSO-d6) δ ppm 8.89 (s, 1H), 8.43 (s, 3H), 8.16 (s, 1H), 6.89 (br s, 1H), 6.54 (br s, 1H), 4.65-4.52 (m, 1H), 4.49-4.32 (m, 2H), 4.17 (br s, 1H), 3.89 (s, 3H), 2.37-2.03 (m, 2H), 1.84 (br s, 3H), 1.63 (br s, 1H). [M+H] calc'd for C17H19F3N6O, 381. found, 381.

1. customan additional 3 h
2. customat 50° C
3. concentrationThe mixture was subsequently concentrated to a dark oil
4. additiondiluted with DMF (1 mL) which
5. customwas purified via preparative HPLC