Sulfuryl chloride → (2Z)-2-(difluoromethoxyimino)-3-oxobutanoic acid
反応式
[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]参加物
4
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-c029835bb377479ebdd048e08b98ff2f
- 出典データセット
- uspto-grants-1990_10
- 特許番号
- US04960766
反応ノート
読み込み中…