Dimethylamine → 4-fluoro-N,N-dimethylbenzenesulfonamide
反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[CH3:12][NH:13][CH3:14]>C(Cl)Cl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:13]([CH3:14])[CH3:12])(=[O:10])=[O:9])=[CH:4][CH:3]=1参加物
4
実験手順
A solution of 38.9 g (0.20 mole) of 4-fluorobenzenesulfonylchloride in 20 ml of methylene chloride was added slowly to 300 ml of a 40% aqueous dimethylamine solution during 0.5 hour period. The reaction was exothermic. After the reaction mixture was cooled a yellow solid was precipitated. The solid was collected, dissolved in 300 ml of ethyl acetate, and dried over magnesium sulfate. The solution was concentrated to 100 ml and a light yellow crystal formed. The crystal was collected and air-dried to afford 39 g of the product, mp 40°-43° C.
後処理
- temperatureAfter the reaction mixture was cooled a yellow solid
- customwas precipitated
- customThe solid was collected
- dissolutiondissolved in 300 ml of ethyl acetate
- dry with materialdried over magnesium sulfate
- concentrationThe solution was concentrated to 100 ml
- customa light yellow crystal formed
- customThe crystal was collected
- customair-dried
出典と根拠
- ORDレコード
- ord-50892e292b354823bf6126a20a71ccd5
- 出典データセット
- uspto-grants-1985_07
- 特許番号
- US04532240
反応ノート
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