Triethylamine → HCID 66593845、化合物
反応式
F[C:2]1[CH:10]=[CH:9][C:8]([CH2:11][C:12]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:15](=[O:22])[NH:14][N:13]=2)=[CH:7][C:3]=1[C:4]([OH:6])=O.[CH2:23]([O:25][CH:26]1[CH2:31][CH2:30][NH:29][CH2:28][CH2:27]1)[CH3:24].C(N(CC)CC)C>CN(C=O)C>[CH2:23]([O:25][CH:26]1[CH2:31][CH2:30][N:29]([C:4]([C:3]2[CH:7]=[C:8]([CH:9]=[CH:10][CH:2]=2)[CH2:11][C:12]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[C:15](=[O:22])[NH:14][N:13]=2)=[O:6])[CH2:28][CH2:27]1)[CH3:24]参加物
5
実験手順
2-(1H-Benzo[d][1,2,3]triazol-1-yl)-1,1,3,3-tetramethylisouronium hexafluorophosphate(V) (0.379 g, 1.00 mmol) was added to 3-((4-oxo-3,4-dihydrophthalazin-1-yl)methyl)benzoic acid (1b) (0.200 g, 0.71 mmol), 4-ethoxypiperidine (0.101 g, 0.78 mmol) and triethylamine (0.249 mL, 1.78 mmol) in DMF (3 mL). The resulting solution was stirred at room temperature for 3 days. The crude product was purified by preparative HPLC (Waters XBridge Prep C18 OBD column, 5μ silica, 19 mm diameter, 100 mm length), using decreasingly polar mixtures of water (containing 1% NH3) and MeCN as eluents. Fractions containing the desired compound were evaporated to dryness to afford the desired compound (0.175 g, 62.6% yield); 1H NMR (400.132 MHz, DMSO) δ 1.11 (3H, t), 1.20-1.93 (4H, m), 2.98-3.27 (2H, m), 3.33-3.41 (1H, m), 3.42-3.54 (3H, m), 3.93 (1H, s), 4.35 (2H, s), 7.21 (1H, m), 7.31 (1H, s), 7.33-7.42 (2H, m), 7.79-7.90 (2H, m), 7.95 (1H, m), 8.26 (1H, m), 12.58 (1H, s); m/z (LC-MS, ESI+), RT=1.81 min (M+H=392.13).