反応式
[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[N:11]=[C:10]([CH3:12])[N:9]([CH2:13][C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[Cl:20])[C:8]=2[CH:21]=1)([OH:3])=O.[N+:22]([C:25]1[CH:30]=[CH:29][C:28]([S:31]([NH2:34])(=[O:33])=[O:32])=[CH:27][CH:26]=1)([O-:24])=[O:23]>CN(C)C=O>[Cl:20][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][C:14]=1[CH2:13][N:9]1[C:8]2[CH:21]=[C:4]([C:1](=[O:3])[NH:34][S:31]([C:28]3[CH:27]=[CH:26][C:25]([N+:22]([O-:24])=[O:23])=[CH:30][CH:29]=3)(=[O:33])=[O:32])[CH:5]=[CH:6][C:7]=2[N:11]=[C:10]1[CH3:12]参加物
実験手順
N,N′-carbonyldiimidazole (0.432 g) is added all at once to an N,N-dimethylformamide (15 ml) solution of 6-carboxy-1-(2-chlorobenzyl)-2-methylbenzimidazole (0.432 g) (example 75), and the solution is stirred for one hour at room temperature. Subsequently, an N,N-dimethylformamide (5 ml) solution of 4-nitrobenzenesulfonamide (0.538 g) and diazabicyclotindecene (0.405 g) is added, and the solution is stirred for 84 hours at 100° C. The reaction solution is cooled and the solvent is removed through evaporation under reduced pressure. When chloroform and hydrochloric acid are added to the residue and the solution is stirred, crystals precipitated. The crystals are separated through filtration, dried, and thus, 1-(2-chlorobenzyl)-2-methyl-6-(4-nitrobenzenesulfonylcarbamoyl)benzimidazole (0.300 g) is obtained.
後処理
- stirringthe solution is stirred for 84 hours at 100° C
- temperatureThe reaction solution is cooled
- customthe solvent is removed through evaporation under reduced pressure
- additionWhen chloroform and hydrochloric acid are added to the residue
- stirringthe solution is stirred
- customcrystals precipitated
- customThe crystals are separated through filtration
- customdried
出典と根拠
- ORDレコード
- ord-08d94b7200534d1ab77db94f0a2fe645
- 出典データセット
- uspto-grants-2002_02
- 特許番号
- US06348032B1
関連ノート
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