反応式
[F:1][C:2]1[C:3]([CH2:15][O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[C:4]([C:8](=O)[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:5]=[CH:6][CH:7]=1.Cl.[O:22]([NH2:24])[CH3:23].C([O-])(=O)C.[Na+]>C(O)C>[F:1][C:2]1[C:3]([CH2:15][O:16][C:17]([CH3:20])([CH3:19])[CH3:18])=[C:4]([C:8](=[N:24][O:22][CH3:23])[C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:5]=[CH:6][CH:7]=1参加物
反応条件
- 温度
- 60 °C
実験手順
To a solution of 79 g (0.28 mole) of ethyl 3-fluoro-2-[(1,1-dimethylethoxy)methyl]-α-oxo-benzeneacetate in 300 mL of ethyl alcohol was added 100 mL (0.39 mole, 30% aq) of methoxylamine HCl followed by 33 g (0.4 mole) of sodium acetate. The mixture was then heated at 60° C. for three hours. After cooling to room temperature, the salts were filtered and the mixture was concentrated in vacuo. Water and EtOAc were added, the layers separated, and the organics were washed with saturated NaHCO3, brine and dried over MgSO4. After filtration, the solution was concentrated in vacuo to give 86.1 g of ethyl 3-fluoro-2-[(1,1-dimethylethoxy)methyl]-α-(methoxyimino)-benzeneacetate as a lightly tinted oil, 1:2 ratio of oxime isomers by gas chromatography.
後処理
- temperatureAfter cooling to room temperature
- filtrationthe salts were filtered
- concentrationthe mixture was concentrated in vacuo
- additionWater and EtOAc were added
- customthe layers separated
- washthe organics were washed with saturated NaHCO3, brine
- dry with materialdried over MgSO4
- filtrationAfter filtration
- concentrationthe solution was concentrated in vacuo
出典と根拠
- ORDレコード
- ord-4dff60d5c90b493f8b75994341426f3e
- 出典データセット
- uspto-grants-1999_10
- 特許番号
- US05968875
関連ノート
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