Sulfuric Acid → 2,6-Difluoro-3-sulfino-benzoic acid
反応式
S([O-])([O-])=O.[Na+].[Na+].Cl[S:8]([C:11]1[C:12]([F:21])=[C:13]([C:17]([F:20])=[CH:18][CH:19]=1)[C:14]([OH:16])=[O:15])(=[O:10])=[O:9].S(=O)(=O)(O)O>O>[F:21][C:12]1[C:11]([S:8]([OH:10])=[O:9])=[CH:19][CH:18]=[C:17]([F:20])[C:13]=1[C:14]([OH:16])=[O:15]参加物
5
実験手順
240 mmol of sodium sulfite were dissolved in 150 ml of water. 32 mmol of 3-Chlorosulfonyl-2,6-difluoro-benzoic acid was added under stirring over a period of about 20 min. After stirring for an additional hour at room temperature, the mixture was chilled and acidified with 20% aqueous sulfuric acid. The product was extracted with ethyl acetate to yield the title compound as a colorless solid. MS (m/e): 221.3 (M−H, 34%)
後処理
- stirringAfter stirring for an additional hour at room temperature
- temperaturethe mixture was chilled
- extractionThe product was extracted with ethyl acetate
出典と根拠
- ORDレコード
- ord-bd3973856463401fa4931b4d83a5f69a
- 出典データセット
- uspto-grants-2009_10
- 特許番号
- US07605163B2
反応ノート
読み込み中…