反应详情

温度

100 °C

A mixture of N-[(1E)-(dimethylamino)methylidene]-4-[3-methyl-1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1(14),2,4,10,12-pentaene-12-carboxamide (100 mg, 0.246 mmol) and 4-hydrazinyl-1-methylpiperidine hydrochloride (81 mg, 0.49 mmol) in acetic acid (10 mL) was heated at 100° C. for 1 h. The solvent was removed under reduce pressure, and the residue was purified by prep-HPLC (Gilson GX 281, Shim-pack PRC-ODS 250 mm×20 mm×2, gradient: CH3CN/10 mm/L NH4HCO3, 17 min) to afford 255 (40 mg, 34% yield) as a white solid. LCMS (ESI): RT=4.28 min, m/z: 474.3 [M+H+]. 1H NMR (500 MHz, DMSO-d6) δ 8.58-8.57 (d, J=8.0 Hz, 1H), 8.08 (s, 1H), 7.99 (s, 1H), 7.44-7.42 (dd, J=8.0, 1.5 Hz, 1H), 7.31 (d, J=1.5 Hz, 1H), 5.86 (m, 1H), 4.58 (s, 4H), 4.31 (m, 1H), 2.86-2.84 (m, 2H), 2.26 (s, 3H), 2.18 (s, 3H), 2.13-2.07 (m, 2H), 2.01-1.96 (m, 2H), 1.91-1.89 (m, 2H), 1.47 (d, J=6.5 Hz, 6H)

1. customThe solvent was removed
2. customthe residue was purified by prep-HPLC (Gilson GX 281, Shim-pack PRC-ODS 250 mm×20 mm×2, gradient: CH3CN/10 mm/L NH4HCO3, 17 min)