反应详情

温度

100 °C

To a solution of (2E)-3-(dimethylamino)-1-{4-[1-(2-hydroxyethyl)-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 (105 mg, 0.270 mmol) in acetic acid (2.0 mL) was added hydrochloric 4-hydrazinyl-1-methylpiperidine (53 mg, 0.32 mmol). The mixture 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 give 257 (17 mg, 13% yield). LCMS (ESI): RT=4.05 min, m/z: 461.2 [M+H+]. 1H NMR (500 MHz, DMSO-d6) δ 8.55 (d, J=8.5 Hz, 1H), 8.10 (s, 1H), 7.94 (s, 1H), 7.55 (d, J=1.5 Hz, 1H), 7.23 (d, J=9 Hz, 1H), 7.11 (s, 1H), 6.40 (d, J=1.5 Hz, 1H), 4.98 (t, J=10.5, 1H), 4.84 (t, J=12, 2H), 4.58 (s, 4H), 4.16 (t, J=23 Hz, 1H), 3.88-3.86 (m, 2H), 2.85 (d, J=10 Hz, 2H), 2.15-2.13 (m, 5H), 1.94 (s, 2H), 1.81 (d, J=11.5, 2H)

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)