4-Nitrophenyl chloroformate → HCID 86670942、化合物
反応式
[C:1](Cl)(=O)[O:2]C1C=CC([N+]([O-])=O)=CC=1.[NH2:14][C:15]1[CH:44]=[CH:43][C:18]([CH:19]=[C:20]2[CH2:25][CH2:24][N:23]([CH2:26][C:27]3[CH:32]=[CH:31][C:30]([C:33]([OH:42])([C:38]([F:41])([F:40])[F:39])[C:34]([F:37])([F:36])[F:35])=[CH:29][CH:28]=3)[CH2:22][CH2:21]2)=[CH:17][CH:16]=1.[NH2:45][CH2:46][C:47]([CH3:50])([OH:49])[CH3:48]>O1CCOCC1>[F:37][C:34]([F:35])([F:36])[C:33]([C:30]1[CH:31]=[CH:32][C:27]([CH2:26][N:23]2[CH2:22][CH2:21][C:20](=[CH:19][C:18]3[CH:17]=[CH:16][C:15]([NH:14][C:1]([NH:45][CH2:46][C:47]([OH:49])([CH3:50])[CH3:48])=[O:2])=[CH:44][CH:43]=3)[CH2:25][CH2:24]2)=[CH:28][CH:29]=1)([OH:42])[C:38]([F:41])([F:39])[F:40]参加物
5
実験手順
4-Nitrophenyl carbonochloridate (0.225 mmol, 45.4 mg) was added to a stirred solution of 2-(4-((4-(4-aminobenzylidene)piperidin-1-yl)methyl)phenyl)-1,1,1,3,3,3-hexafluoropropan-2-ol (0.225 mmol, 100 mg) in dioxane (1 mL) and the mixture stirred at room temperature for 1 hour. 1-Amino-2-methylpropan-2-ol (0.675 mmol, 60.2 mg) was added and the mixture stirred at room temperature for 1.5 hours. The mixture was washed with water (1 mL), the organic phase dried over magnesium sulfate, filtered and concentrated under reduced pressure. The resulting residue was purified by HPLC and treated with strong cation exchange column to afford the title compound (17 mg). MS (ESI) m/z 560.2 [M+H]+