Ammonia → 4,4-Dimethylpentane-1-sulfonamide
反応式
[NH3:1].[CH3:2][C:3]([CH3:12])([CH3:11])[CH2:4][CH2:5][CH2:6][S:7](Cl)(=[O:9])=[O:8]>O1CCCC1>[CH3:2][C:3]([CH3:12])([CH3:11])[CH2:4][CH2:5][CH2:6][S:7]([NH2:1])(=[O:9])=[O:8]参加物
4
実験手順
Anhydrous ammonia gas was passed into a solution of 4,4-dimethylpentane sulphonyl chloride (1.85 g) in dry tetrahydrofuran (5 ml) at 5-10° C. until saturation. The resulting suspension was stirred at room temperature for 18 hours and then evaporated under reduced pressure. The residue was partitioned between ethyl acetate (20 ml) and 2N aqueous hydrochloric acid (20 ml). The organic phase was separated, washed (brine 20 ml), dried (Na2SO4) and evaporated. Column chromatography on silica eluting with dichloromethane:methanol 98:2 gave 4,4-dimethylpentane sulphonic acid amide as an off-white solid (0.72 g).
後処理
- customevaporated under reduced pressure
- customThe residue was partitioned between ethyl acetate (20 ml) and 2N aqueous hydrochloric acid (20 ml)
- customThe organic phase was separated
- washwashed (brine 20 ml)
- dry with materialdried (Na2SO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-53f60ff02f1a4e9892e5b6138e9d2412
- 出典データセット
- uspto-grants-2003_08
- 特許番号
- US06610518B2
反応ノート
読み込み中…