反应详情

3-chloro-5-{[1-({1-(4-methoxybenzyl)-6-[(4-methoxybenzyl)amino]-1H-pyrazolo[3,4-b]pyridin-3-yl}methyl)-2-oxo-4-(trifluoromethyl)-1,2-dihydropyridin-3-yl]oxy}benzonitrile (0.185 g, 0.264 mmol) was dissolved in TFA (5 mL) and placed in an oil bath at 75° C. After 2 hours, the reaction mixture was concentrated under reduced pressure and purified by preparative HPLC eluting with 30-95% MeCN/H2O+0.1% TFA to afford the title compound as a solid. 1H NMR (DMSO-d6, with NH4OH) δ 7.94 (d, J=7.3 Hz, 1H), 7.77-7.74 (m, 1H), 7.62-7.56 (m, 2H), 7.50-7.46 (m, 1H), 6.60 (d, J=7.3 Hz, 1H), 6.38-6.33 (m, 2H), 6.30 (d, J=8.8 Hz, 1H), 5.32 (s, 2H). HRMS (M+1)=461.0729.

1. customplaced in an oil bath at 75° C
2. concentrationthe reaction mixture was concentrated under reduced pressure
3. custompurified by preparative HPLC
4. washeluting with 30-95% MeCN/H2O+0.1% TFA