反应详情

N2-[4-(4-amino-1-{1-[(2-methyl-1H-4-imidazolyl)methyl]-4-piperidyl}-1H-pyrazolo[3,4-d]pyrimidin-3-yl)-2-methoxyphenyl]-1-methyl-1H-2-indolecarboxamide (210 mg, 0.355 mmol) was dissolved in hot ethyl acetate (25 mL) and a few drops of ethanol. Maleic acid (83 mg, 0.711 mmol) in hot ethyl acetate (3 mL) was added. The reaction mixture was stirred at room temperature for 3 hours. The solid was collected by filtration to give N2-[4-(4-amino-1-{1-[(2-methyl-1H-4-imidazolyl)methyl]-4-piperidyl}-1H-pyrazolo[3,4-d]pyrimidin-3-yl)-2-methoxyphenyl]-1-methyl-1H-2-indolecarboxamide, dimaleate salt (255 mg, 87%). 1H NMR (DMSO-d6) δ 2.12 (m, 2H), 2.43 (m, 5H), 2.92 (m, 2H), 3.38 (m, 2H), 3.96 (s, 3H), 3.99 (s, 2H), 4.04 (s, 3H), 4.93 (m, 1H), 6.13 (s, 4H), 7.16 (m, 1H), 7.34 (m, 5H), 7.60 (d, J=8.43 Hz, 1H), 7.70 (d, J=7.92 Hz, 1H), 7.72 (d, J=8.15 Hz, 1H), 8.27 (s, 1H), 9.44 (s, 1H). LCMS (Thermoquest AQA single Quad MS, Finnigan HPLC-Column: Genesis, C18, 3 um, 33×4.6 mm. Eluents: 30% B/A to 95% B/A in 4.5 min. (B: acetonitrile, A: 50 mM ammonia acetate buffer, PH 4.5), 0.8 mL/min.): RT=1.98 min. MH+=591.3.

1. filtrationThe solid was collected by filtration