Sulfuryl chloride → (2Z)-2-(difluoromethoxyimino)-3-oxobutanoic acid
반응식
[F:1][CH:2]([F:16])[O:3][N:4]=[C:5]([C:13](=[O:15])[CH3:14])[C:6]([O:8]C(C)(C)C)=[O:7].S(Cl)(Cl)(=O)=O>C(O)(=O)C>[F:1][CH:2]([F:16])[O:3]/[N:4]=[C:5](/[C:13](=[O:15])[CH3:14])\[C:6]([OH:8])=[O:7]참가 물질
4
실험 절차
To a solution of tert-butyl 2-difluoromethoxyimino-3-oxobutyrate (9.4 g) in acetic acid (9.4 ml) was added sulfuryl chloride (2.55 ml) under ice-cooling. After stirred at ambient temperature for an hour, the reaction mixture was concentrated under reduced pressure. The residual oil was dissolved in ethyl acetate. The ethyl acetate solution was washed with water, dried over magnesium sulfate, and evaporated in vacuo. The residue was crystallized with diisopropyl ether to give (Z)-2-difluoromethoxyimino-3-oxobutyric acid (4.73 g).
후처리
- temperaturecooling
- concentrationthe reaction mixture was concentrated under reduced pressure
- dissolutionThe residual oil was dissolved in ethyl acetate
- washThe ethyl acetate solution was washed with water
- dry with materialdried over magnesium sulfate
- customevaporated in vacuo
- customThe residue was crystallized with diisopropyl ether
출처 및 근거
- ORD 기록
- ord-c029835bb377479ebdd048e08b98ff2f
- 출처 데이터셋
- uspto-grants-1990_10
- 특허 번호
- US04960766
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