反应详情

A mixture of 4-[3-methyl-1-(propan-2-yl)-1H-1,2,4-triazol-5-yl]-12-[1-methyl-5-(piperidin-3-yl)-1H-pyrazol-4-yl]-9-oxa-3,6-diazatricyclo[8.4.0.02,6]tetradeca1 (14),2,4,10,12-pentaene (80 mg, 0.17 mmol), tetrahydropyran-4-one (25 mg, 0.25 mmol) and Ti(O-iPr)4 (2 drops) in EtOH (20 mL) was stirred at room temperature for 18 h. After concentration, 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 give 213 (16 mg, 18% yield). LCMS (ESI): RT=4.75 min, m/z: 527.3 [M+H+]. 1H NMR (500 MHz, DMSO-d6) δ 8.42 (d, J=8.0 Hz, 1H), 7.91 (s, 1H), 7.43 (s, 1H), 7.08 (d, J=1.5 Hz, 1H), 6.94 (s, 1H), 7.39-7.36 (m, 1H), 5.87-5.84 (m, 1H), 4.54-4.40 (m, 8H), 3.90 (s, 3H), 3.18 (s, 1H), 2.74-2.69 (m, 2H), 2.24 (s, 3H), 2.11-2.06 (m, 1H), 1.78-1.71 (m, 5H), 1.47 (d, J=2.0 Hz, 6H)

1. concentrationAfter concentration
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)