Acetic Anhydride → HCID 89963113、化合物

反応式

[Cl:1][C:2]1[C:3]([O:19][C@H:20]2[CH2:25][CH2:24][C@@H:23]([OH:26])[CH2:22][C@@H:21]2[C:27]2[N:31]([CH3:32])[N:30]=[CH:29][CH:28]=2)=[CH:4][C:5]([F:18])=[C:6]([S:8]([NH:11][C:12]2[CH:17]=[CH:16][N:15]=[CH:14][N:13]=2)(=[O:10])=[O:9])[CH:7]=1.[C:33](OC(=O)C)(=[O:35])[CH3:34]>CN(C1C=CN=CC=1)C.N1C=CC=CC=1>[C:33]([O:26][C@@H:23]1[CH2:24][CH2:25][C@H:20]([O:19][C:3]2[CH:4]=[C:5]([F:18])[C:6]([S:8](=[O:10])(=[O:9])[NH:11][C:12]3[CH:17]=[CH:16][N:15]=[CH:14][N:13]=3)=[CH:7][C:2]=2[Cl:1])[C@@H:21]([C:27]2[N:31]([CH3:32])[N:30]=[CH:29][CH:28]=2)[CH2:22]1)(=[O:35])[CH3:34]

参加物

実験手順

A solution of the 5-chloro-2-fluoro-4-{[(1S,2R,4R)-4-hydroxy-2-(1-methyl-1H-pyrazol-5-yl)cyclohexyl]oxy}-N-(pyrimidin-4-yl)benzenesulfonamide (22.0 mg, 0.046 mmol) prepared in Example 165d, acetic anhydride (0.50 mL) and 4-(N,N-dimethylamino)pyridine (0.6 mg, 0.0046 mmol) in pyridine (1.0 mL) was stirred at room temperature for 3 hours. The reaction solution was concentrated, and 1 M HCl (10 mL) was then added to the residue, followed by extraction with dichloromethane (50 mL). The thus obtained organic layer was dried over anhydrous sodium sulfate. After vacuum concentration, the residue was purified with silica gel chromatography (dichloromethane/methanol=10:1) to yield the title compound (22.0 mg, 91%) as a colorless solid.