Oxalyl chloride → HCID 86639365、化合物

反応式

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

参加物

反応条件

温度: 0 °C

実験手順

To a suspension of 5-fluoro-1-{[2-(3-fluorophenyl)-4-methylpyrimidine-5-carbonyl]amino}-1H-indole-3-sulfonic acid (1.06 g) in DCM (60 mL) at 0° C. is added dry DMF (10 drops). Oxalyl chloride (1.05 mL) is added drop wise and the mixture is stirred at 0° C. for 3 h. The mixture is filtered and the collected solid is washed with ether to afford 5-fluoro-1-{[2-(3-fluorophenyl)-4-methylpyrimidine-5-carbonyl]amino}-1H-indole-3-sulfonyl chloride (0.94 g). MS: 461 (M−H)