関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | O-Methylhydroxylamine hydrochloride | HCID 521874 | — |
| 反応物 | Ethyl 3-fluoro-2-[(1,1-dimethylethoxy)methyl]-alpha-oxo-benzeneacetate | HCID 21836286 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl 3-fluoro-2-[(1,1-dimethylethoxy)methyl]-alpha-(methoxyimino)-benzeneacetate | HCID 53693715 | 98.8% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05968875 |
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| 出典データセット | uspto-grants-1999_10 |
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| ORD ID | ord-4dff60d5c90b493f8b75994341426f3e |
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| 出典メモ | uspto-grants-1999_10 |
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