反応式
[C:1]1([CH3:13])[C:2]([S:7]([N:10]=[C:11]=[O:12])(=[O:9])=[O:8])=[CH:3][CH:4]=[CH:5][CH:6]=1.[CH3:14][C:15]1[CH:16]=[C:17]([CH:19]=[C:20]([CH3:29])[C:21]=1[S:22]([CH2:25][N+:26]([O-:28])=[O:27])(=[O:24])=[O:23])[NH2:18]>C(Cl)Cl>[CH3:29][C:20]1[CH:19]=[C:17]([NH:18][C:11]([NH:10][S:7]([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=2[CH3:13])(=[O:9])=[O:8])=[O:12])[CH:16]=[C:15]([CH3:14])[C:21]=1[S:22]([CH2:25][N+:26]([O-:28])=[O:27])(=[O:24])=[O:23]参加物
4
実験手順
A solution of 0.77 ml (5.09 mmol) of o-toluenesulphonyl isocyanate in 7.7 ml of anhydrous methylene chloride is added dropwise to a suspension, maintained under a nitrogen atmosphere, of 1.3 g (5.32 mmol) of 3,5-dimethyl-4-[(nitromethyl)sulphonyl]aniline in 25.6 ml of anhydrous methylene chloride. The temperature of the reaction medium rises spontaneously by 7° C. A precipitate forms in the solution initially obtained. Stirring is continued for 1 hour at room temperature and the solid is then isolated by filtration and washed with hexane to give 1.9 g (yield=86%) of 1-[3,5-dimethyl-4-[(nitromethyl)sulphonyl]phenyl]-3-[(2-methylphenyl)sulphonyl]urea.
後処理
- customrises spontaneously by 7° C
- customA precipitate forms in the solution initially obtained
- customthe solid is then isolated by filtration
- washwashed with hexane
出典と根拠
- ORDレコード
- ord-eb98b86be4084b87bec67089f8d78ed8
- 出典データセット
- uspto-grants-2003_01
- 特許番号
- US06509499B1
関連ノート
読み込み中…