Cesium carbonate → HCID 66669839、化合物
反応式
[F:1][C:2]1[CH:3]=[C:4]([N:20]([C:29]2[CH:34]=[CH:33][C:32]([F:35])=[CH:31][CH:30]=2)[C:21]([C:23]2([C:26]([NH2:28])=[O:27])[CH2:25][CH2:24]2)=[O:22])[CH:5]=[CH:6][C:7]=1[O:8][C:9]1[C:18]2[C:13](=[CH:14][C:15]([OH:19])=[CH:16][CH:17]=2)[N:12]=[CH:11][CH:10]=1.[OH:36][CH:37]1[C:41]2([CH2:43][CH2:42]2)[CH2:40][N:39]([CH2:44][CH2:45][CH2:46]CS([O-])(=O)=O)[CH2:38]1.C([O-])([O-])=O.[Cs+].[Cs+]>CC(N(C)C)=O>[OH:36][CH:37]1[C:41]2([CH2:43][CH2:42]2)[CH2:40][N:39]([CH2:44][CH2:45][CH2:46][O:19][C:15]2[CH:14]=[C:13]3[C:18]([C:9]([O:8][C:7]4[CH:6]=[CH:5][C:4]([N:20]([C:29]5[CH:30]=[CH:31][C:32]([F:35])=[CH:33][CH:34]=5)[C:21]([C:23]5([C:26]([NH2:28])=[O:27])[CH2:25][CH2:24]5)=[O:22])=[CH:3][C:2]=4[F:1])=[CH:10][CH:11]=[N:12]3)=[CH:17][CH:16]=2)[CH2:38]1参加物
5
実験手順
To a solution of N-(3-fluoro-4-(7-hydroxy-quinolin-4-yloxy)phenyl)-N-(4-fluorophenyl)cyclopropane-1,1-dicarboxamide (266 mg, 0.56 mmol) in DMA (3 mL) was added 3-(7-hydroxy-5-azaspiro[2.4]heptane-5-yl)propylmethanesulfonate (283 mg, 1.14 mmol) and Cs2CO3 (556 mg, 1.71 mmol). The reaction was then stirred at rt for 2 days. The solvent was then removed and the residue was partioned between saturated NaHCO3 aqueous solution (15 mL) and CHCl3 (30 mL). The organic layer was separated, dried over anhydrous Na2SO4, filtered. The filtrate was concentrated in vacuo. The residue was purified by a silica gel column chromatography (100:15:1(v/v/v) EtOAc/CH3OH/Et3N) to afford the title compound as a white solid (290 mg, 82%).