反应详情

trans-N2-(4-{4-Amino-1-[4-(4-methylpiperazino)cyclohexyl]-1H-pyrazolo[3,4-d]pyrimidin-3-yl}-2-methoxyphenyl)benzo[b]furan-2-carboxamide (497 mg, 0.855 mmol) was dissolved in hot ethyl acetate (56 mL) and maleic acid (298mg, 2.566 mmol) in hot ethyl acetate (5 mL) was added. The reaction mixture was stirred at room temperature for 5 hours. The solid was collected by filtration to give trans-N2-(4-{4-Amino-1-[4-(4-methylpiperazino)cyclohexyl]-1H-pyrazolo[3,4-d]pyrimidin-3-yl}-2-methoxyphenyl)benzo[b]furan-2-carboxamide, trimaleate salt (117 mg, 92%). 1H NMR (DMSO-d6) δ 1.60 (m, 2H), 2.09 (m, 6H), 2.68 (s, 3H), 2.82-3.17 (bm, 9H), 4.00 (s, 3H), 4.69 (m, 1H), 6.16 (s, 6H), 7.30-7.42 (m, 3H), 7.54 (m, 1H), 7.76-7.85 (m, 3H), 8.25 (m, 2H), 9.51 (s, 1H); LCMS (Finigan-Column: Pecosphere, C18, 3 um, 33×4.6 mm. Eluents: 0% B/A to 100% B/A in 4 min. (B: acetonitrile, A: 50 mM ammonia acetate buffer, pH 4.5), 3.0 mL/min.): MH+ =581.4, Rt=2.12 min.

1. filtrationThe solid was collected by filtration