反应详情

To mixture of 2-hydroxy-5-(2-methoxy-pyridin-3-yl)-benzaldehyde (57 mg, 0.25 mmol) and 3-(4-methyl-piperazin-1-yl)-benzene-1,2-diamine (51 mg, 0.25 mol) was added DMA (1 mL) and the resulting solution was stirred at the room temperature for 15 min, heated at 110° C. for 15 h open to the air, concentrated under reduced pressure. The residual crude was purified by chromatography (500:10:1 CH2Cl2/MeOH/28% aqueous NH4OH) to afford the title compound (10.8 mg, 10.5%). 1H NMR (MeOH-d4) δ 2.41 (s, 3H), 2.78 (m, 4H), 3.49 (m, 4H), 3.97 (s, 3H), 6.72 (m, 1H) 7.05-7.20 (4H), 7.56 (d, J=9 Hz, 1H), 7.78 (d, J=9 Hz, 1H), 8.10-8.13 (2H). ESI-MS m/z 416.5 (MH+).

1. temperatureheated at 110° C. for 15 h open to the air
2. concentrationconcentrated under reduced pressure
3. customThe residual crude was purified by chromatography (500:10:1 CH2Cl2/MeOH/28% aqueous NH4OH)