反应详情

6-Chloro-2-fluoro-N-(3-methoxy-1-(4-methoxybenzyl)-1H-pyrazolo[3,4-b]pyridin-5-yl)-3-(propylsulfonamido)benzamide (0.027 g, 0.0480 mmol) was heated to reflux in TFA overnight. The reaction mixture was cooled to room temperature and was concentrated to an oil. DCM was added to the oil resulting in a precipitate, which was collected by filtration giving 6-chloro-2-fluoro-N-(3-methoxy-1H-pyrazolo[3,4-b]pyridin-5-yl)-3-(propylsulfonamido)benzamide (0.0175 g, 82%) as a solid. 1H NMR (400 MHz, d6-DMSO) δ 12.60 (s, 1H), 11.07 (1H, s), 9.99 (br s, 1H), 8.58 (s, 1H), 8.49 (s, 1H), 7.52-7.57 (m, 1H), 7.44-7.46 (m, 1H), 4.02 (s, 3H), 3.15-3.19 (m, 2H), 1.73-1.79 (m, 2H), 0.97-1.01 (m, 3H); m/z (APCI-pos) M+1=442.1.

1. concentrationwas concentrated to an oil
2. additionDCM was added to the oil
3. customresulting in a precipitate, which
4. filtrationwas collected by filtration