反应详情

At 0° C., 3-[5-(4-chloro-phenyl)-4-oxo-6-(4-pyrazin-2-yl-phenyl)-4,5-dihydro-pyrazolo[3,4-d]pyrimidin-1-yl]-benzonitrile (prepared as described in example 47, 0.65 g, 1.29 mmol) is added to methanol saturated with hydrogen chloride gas (20 mL) with stirring. The reaction mixture is allowed to reach rt and stirred there for 40 h. The reaction mixture is then concentrated to a dry residue (0.7 g). It is taken in dry methanol (40 mL) and ammonium carbonate (1.15 g, 7.36 mmol) is added. After stirring at rt for 40 h, the reaction mixture is concentrated and the residue obtained is purified by column chromatography to afford 3-[5-(4-chloro-phenyl)-4-oxo-6-(4-pyrazin-2-yl-phenyl)-4,5-dihydro-pyrazolo[3,4-d]pyrimidin-1-yl]-benzamidine. 1H NMR (DMSO-d6, 400 MHz) δ 9.25 (s, 1H), 8.71 (s, 1H), 8.63 (m, 1H), 8.55 (m, 2H), 8.29 (dd, 1H), 8.16 (s, 1H), 8.07 (m, 1H), 7.90 (m, 1H), 7.67 (m, 1H), 7.62 (m, 2H), 7.52 (m, 1H), 7.44 (m, 4H); LC-MS calculated for C28H19ClN8O (M+H+) 519.1, found 519.9.

1. customto reach rt
2. stirringstirred there for 40 h
3. concentrationThe reaction mixture is then concentrated to a dry residue (0.7 g)
4. stirringAfter stirring at rt for 40 h
5. concentrationthe reaction mixture is concentrated
6. customthe residue obtained
7. customis purified by column chromatography