Acetic Acid → 4-Chloro-3-fluoro-2-methylsulphonylbenzoic acid
반응식
OO.[Cl:3][C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[C:6](SC)[C:5]=1[F:15].[S:16](=[O:20])(=O)(O)[OH:17].S(S([O-])=O)([O-])(=O)=O.[Na+].[Na+].[C:30](O)(=O)C>>[Cl:3][C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[C:6]([S:16]([CH3:30])(=[O:20])=[O:17])[C:5]=1[F:15]참가 물질
6
반응 조건
- 온도
- 80 °C
실험 절차
Hydrogen peroxide (30%; 66 ml) was added to a suspension of 4-chloro-3-fluoro-2-(methylsulphenyl)benzoic acid (2.5 g) and concentrated sulphuric acid (1.5 ml) in acetic acid. The mixture was heated slowly to 80° C. and stirred and heated at that temperature overnight. It was cooled to room temperature and treated with sodium metabisulphite (45 g). It was evaporated and the residue was treated with water and acidified to pH 1. It was extracted with ethyl acetate, washed with water, dried (MgSO4) and filtered. The filtrate was evaporated to dryness to give 4-chloro-3-fluoro-2-methylsulphonylbenzoic acid (24 g) as an off white solid m.p. 196°-200° C.
후처리
- temperatureheated at that temperature overnight
- temperatureIt was cooled to room temperature
- customIt was evaporated
- additionthe residue was treated with water
- extractionIt was extracted with ethyl acetate
- washwashed with water
- dry with materialdried (MgSO4)
- filtrationfiltered
- customThe filtrate was evaporated to dryness
출처 및 근거
- ORD 기록
- ord-0c8b08f3d48c42778baea2591b7f3287
- 출처 데이터셋
- uspto-grants-1994_12
- 특허 번호
- US05371064
반응 노트
불러오는 중…