反応式
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH3:6][N:7]([CH3:15])[C:8]1[CH:13]=[CH:12][CH:11]=[C:10]([NH2:14])[CH:9]=1.[OH-].[Na+]>O>[CH3:6][N:7]([CH3:15])[C:8]1[CH:9]=[C:10]([NH:14][S:2]([CH3:1])(=[O:4])=[O:3])[CH:11]=[CH:12][CH:13]=1参加物
5
実験手順
Methanesulphonyl chloride (838 mg, 7.35 mmol) was added slowly to a cooled solution (5° C.) of N,N-dimethyl-1,3-phenylenediamine (1.00 g, 7.35 mmol) and sodium hydroxide (5M, 1.5 cm3) in water (10 cm3). The reaction was allowed to warm to room temperature overnight. The mixture was extracted with chloroform (3×15 cm3). The combined extracts were dried over sodium sulphate, filtered and the solvent removed under reduced pressure. Column chromatography (1:20 methanol/dichloromethane) gave the target material as a brown oil (1.24 g, 79%).
後処理
- extractionThe mixture was extracted with chloroform (3×15 cm3)
- dry with materialThe combined extracts were dried over sodium sulphate
- filtrationfiltered
- customthe solvent removed under reduced pressure
出典と根拠
- ORDレコード
- ord-b8fd1201b5654d798122c4747976812a
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08658665B2
関連ノート
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