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-(trifluoromethyl)benzamide (510 mg, 0.838 mmol) was dissolved in hot ethyl acetate (55 mL) and maleic acid (292 mg, 2.513 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 trans-N1-(4-{4-amino-1-[4-(4-methylpiperazino)cyclohexyl]-1H-pyrazolo[3,4-d]pyrimidin-3-yl}-2-methoxyphenyl)-4-(trifluoromethyl)benzamide, dimaleate salt (802 mg, 100%). 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), 6.17 (s, 6H), 7.29 (d, J=8.12 Hz, 1H), 7.33 (s, 1H), 7.92 (d, J=8.34 Hz, 2H), 8.02 (d, J=8.12 Hz, 1H), 8.17 (d, J=8.12 Hz, 2H), 8.26 (s, 1H), 9.83 (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+ =609.4, Rt=2.16 min.

1. filtrationThe solid was collected by filtration trans-N1-(4-{4-amino-1-[4-(4-methylpiperazino)cyclohexyl]-1H-pyrazolo[3,4-d]pyrimidin-3-yl}-2-methoxyphenyl)-4-(trifluoromethyl)benzamide, dimaleate salt (802 mg, 100%)
2. waitEluents: 0% B/A to 100% B/A in 4 min. (B