[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1Cl.C(=O)([O-])[O-].[Na+].[Na+].[N:16]1([CH2:22][CH2:23][OH:24])[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1>CN(C)C(=O)C>[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[N:19]1[CH2:20][CH2:21][N:16]([CH2:22][CH2:23][OH:24])[CH2:17][CH2:18]1In a 50 mL round bottom flask, 9.18 g (0.05 mol) of 3,4,6-trichloro-pyridazine, 5.30 g (0.05 mol) of anhydrous sodium carbonate and 20 mL of N,N-dimethylacetamide (DMA) were added, stirred at room temperature, then 6.54 g (0.05 mol) of 2-(piperazin-1-yl)-ethanol (dissolved in 10 ml DMA) was added dropwise slowly, stirred overnight, filtered on the next day. 100 mL of distilled water was added into the filter cake and stirred, then filtered again to obtain 10.20 g of a white solid, yield: 73.6%, m.p. 139˜141° C. 1H-NMR(400 MHz, CDCl3) δppm: 2.57(br, 1H), 2.66˜2.68(t, 2H, J=5.12 Hz), 2.73˜2.76(t, 4H, J=4.76 Hz), 3.36˜3.38(t, 4H, J=4.52 Hz), 3.68˜3.71(t, 2H, J=5.04 Hz), 6.88(s, 1H). 13C-NMR(400 MHz, DMSO-d6) δppm: 155.14, 149.43, 148.70, 116.64, 60.00, 58.49, 52.44, 48.90.
Wird geladen…
