Dimethylamine → HCID 9400787、化合物
反応式
Cl[C:2]1[N:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1.[CH3:12][NH:13][CH3:14]>>[CH3:12][N:13]([CH3:14])[C:2]1[N:7]=[CH:6][C:5]([S:8]([NH2:11])(=[O:10])=[O:9])=[CH:4][CH:3]=1参加物
3
実験手順
A mixture of 6-chloropyridine-3-sulfonamide (5 g, 0.0259 mol) and aqueous dimethylamine (100 ml, 40%) is stirred at rt for 13 h. The mixture is concentrated to ⅕th of its original volume and cooled. The precipitate is collected by filtration, washed with ice-cold water (10 ml) and dried under vacuum to afford 4.5 g (95%) of the title compound as a solid. mp: 133-138° C., LC/MS: (ES+) 201.9.
後処理
- concentrationThe mixture is concentrated to ⅕th of its original volume
- temperaturecooled
- filtrationThe precipitate is collected by filtration
- washwashed with ice-cold water (10 ml)
- customdried under vacuum
出典と根拠
- ORDレコード
- ord-935b86e1ffc74c7480aee697219bdd08
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08877757B2
反応ノート
読み込み中…