Potassium Carbonate → HCID 21082088、化合物
反応式
[Br-].[NH2:2][C:3]1[CH:12]=[C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[C:15]([Cl:19])[CH:14]=2)[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([CH:20]([C:27]3[CH:32]=[CH:31][C:30]([Cl:33])=[CH:29][CH:28]=3)[C:21]3[N:25]([CH3:26])[CH:24]=[N:23][N:22]=3)[CH:9]=2)[N+:4]=1[CH2:34][C:35](=O)[C:36]([O:38][CH2:39][CH3:40])=[O:37].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[Cl:19][C:15]1[CH:14]=[C:13]([C:11]2[C:10]3[C:5](=[CH:6][CH:7]=[C:8]([CH:20]([C:27]4[CH:28]=[CH:29][C:30]([Cl:33])=[CH:31][CH:32]=4)[C:21]4[N:25]([CH3:26])[CH:24]=[N:23][N:22]=4)[CH:9]=3)[N:4]3[CH:34]=[C:35]([C:36]([O:38][CH2:39][CH3:40])=[O:37])[N:2]=[C:3]3[CH:12]=2)[CH:18]=[CH:17][CH:16]=1参加物
4
実験手順
A mixture of intermediate (67) (0.0006 mol), obtained in Example A12 g, in ethanol (3 ml) was stirred and refluxed for 18 hours. Potassium carbonate 10% was added. The mixture was extracted with DCM. The organic layer was separated, dried (MgSO4), filtered, and the solvent was evaporated till dryness. The residue (0.3 g) was purified by column chromatography over kromasil (eluent: CH2Cl2 100 to CH2Cl2/CH3OH 90/10; 10 μm). The pure fractions were collected and the solvent was evaporated. The residue (0.12 g, 33%) was crystallized from CH3CN/DIPE. The precipitate was filtered off and dried, yielding 0.091 g (25%) of ethyl 5-(3-chlorophenyl)-7-[(4-chlorophenyl)(4-methyl-4H-1,2,4-triazol-3-yl)methyl]-imidazo[1,2-a]quinoline-2-carboxylate, mp. 220° C.