反应详情

2,6-Difluoro-N-(3-methoxy-1-(4-methoxybenzyl)-1H-pyrazolo[3,4-b]pyridin-5-yl)-3-(propylsulfonamido)benzamide (0.0030 g, 0.0055 mmol) was taken up in TFA (2 mL) and heated to reflux for 8 hours. The reaction mixture was concentrated and purified by column chromatography (1:1 hexane/EtOAc) to provide 2,6-difluoro-N-(3-methoxy-1H-pyrazolo[3,4-b]pyridin-5-yl)-3-(propylsulfonamido)benzamide (0.0021 g, 90%) as a solid. 1H NMR (400 MHz, (CD3)2CO) δ 8.65-8.66 (m, 2H), 7.65-7.71 (m, 1H), 7.15-7.20 (m, 1H), 4.07 (s, 3H), 3.16-3.19 (m, 2H), 1.84-1.90 (m, 2H), 1.03-1.07 (m, 3H); m/z (APCI-pos) M+1=426.1.

1. temperatureheated
2. temperatureto reflux for 8 hours
3. concentrationThe reaction mixture was concentrated
4. custompurified by column chromatography (1:1 hexane/EtOAc)