反应详情

温度

100 °C

A mixture of (2E)-3-(dimethylamino)-1-{13-methyl-4-[1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca-1(14),2,4,10,12-pentaen-12-yl}prop-2-en-1-one (110 mg, 0.30 mmol) and 4-hydrazinyl-1-methylpiperidine hydrochloride (42 mg, 0.24 mmol) in acetic acid (2.0 mL) was stirred at 100° C. for 1 hour under nitrogen atmosphere. After concentration, the residue was purified by preparative HPLC (Gilson GX 281, Shim-pack PRC-ODS 250 mm×20 mm×2, gradient: CH3CN/10 mm/L NH4HCO3, 17 min) to afford 264 (30 mg, 21% yield). LCMS (ESI): RT=5.04 min, m/z: 473.3 [M+H+]. 1H NMR (500 MHz, DMSO-d6) δ 8.35 (s, 1H), 8.00 (s, 1H), 7.94 (s, 1H), 7.58 (d, J=1.5 Hz, 1H), 6.92 (s, 1H), 6.27-6.26 (m, 1H), 5.85 (t, J=13 Hz, 1H), 4.55 (t, J=20 Hz, 4H), 3.76 (s, 1H), 2.86 (s, 2H), 2.19-2.11 (m, 8H), 1.78 (s, 2H), 1.74 (d, J=14.5 Hz, 2H), 4.51 (d, J=7 Hz, 6H)

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