反应详情

To a mixture of N2-(4-{4-amino-1-[2-(4-methylpiperazino)ethyl]-1H-pyrazolo[3,4-d]pyrimidin-3-yl}-2-methoxyphenyl)-1-methyl-1H-2-indolecarboxamide (0.082 g, 0.15 mmol) in warm ethyl acetate (2 mL) was added a solution of maleic acid (0.053 g, 0.46 mmol) in warm ethyl acetate (1 mL). A precipitate formed immediately. The reaction mixture was allowed to cool to ambient temperature and the precipitate was collected by filtration, washed with ethyl acetate (5 mL), and dried in vacuo to afford N2-(4-{4-amino-1-[2-(4-methylpiperazino)ethyl]-1H-pyrazolo[3,4-d]pyrimidin-3-yl}-2-methoxyphenyl)-1-methyl-1H-2-indolecarboxamide trimaleate as a beige solid (0.090 g, 0.10 mmol): 1H NMR (d6-DMSO, 400 MHz): δH 9.45 (1H, s), 8.27 (1H, s), 8.12 (1H, d, J=8.0 Hz), 7.71 (1H, d, J=8.0 Hz), 7.59 (1H, d, J=8.0 Hz), 7.29-7.36 (4H, m), 7.15 (1H, t, J=7.4 Hz), 6.17 (6H, s), 4.50 (2H, t, J=6.4 Hz), 4.04 (3H, s), 3.96 (3H, s), 3.10-3.20 (4H, m), 2.92-2.95 (4H, m), 2.74 (3H, s), and 2.32-2.37 (2H, m); RP-HPLC (Hypersil C18, 5 μm, 100 Å, 15 cm; 5%-100% acetonitrile-0.1 M ammonium acetate over 15 min, 1 mL/min). Rt 10.48 min. MS: M+ 540.3.

1. customA precipitate formed immediately
2. filtrationthe precipitate was collected by filtration
3. washwashed with ethyl acetate (5 mL)
4. customdried in vacuo