反应详情

trans-N1-(4-{4-amino-1-[4-(4-methylpiperazino)cyclohexyl]-1H-pyrazolo[3,4-d]pyrimidin-3-yl}-2-methoxyphenyl)-4-(trifluoromethoxy)benzamide (520 mg, 0.832 mmol) was dissolved in hot ethyl acetate (55 mL) and maleic acid (290 mg, 2.497 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-N1-(4-{4-amino-1-[4-(4-methylpiperazino)cyclohexyl]-1H-pyrazolo[3,4-d]pyrimidin-3-yl}-2-methoxyphenyl)-4-(trifluoromethoxy)benzamide, dimaleate salt (780 mg, 96%). 1H NMR (DMSO-d6) δ 1.60 (m, 2H), 2.06 (m, 6H), 2.68 (s, 3H), 2.83-3.17 (bm, 9H), 3.93 (s, 3H), 4.72 (m, 1H), 6.18 (s, 6H), 7.28 (d, J=8.14 Hz, 1H), 7.33 (s, 1H), 7.54 (d, J=8.47 Hz, 2H), 8.01 (d, J=8.12 Hz, 1H), 8.10 (d, J=8.69 Hz, 2H), 8.26 (s, 1H), 9.69 (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+ =625.4, Rt=2.21 min.

1. filtrationThe solid was collected by filtration