関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydroxylamine, sulfate (1:1) | HCID 159255 | — |
| 反応物 | N-methyl-2-(2-phenoxyphenyl)-2-oxoacetamide | HCID 11780091 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | (E)-2-(Hydroxyimino)-N-methyl-2-(2-phenoxyphenyl)acetamide | HCID 9816878 | 95.6% |
反応手順
N-Methyl-2-(2-phenoxyphenyl)-2-oxoacetamide (2.55 g, 10 mmol) was dissolved in methyl alcohol (10 ml). Hydroxylamine sulfate (0.99 g, 12 mmol) was added, followed by heating under reflux for 3 hours. After completion of the reaction, methyl alcohol was evaporated under reduced pressure. Toluene (10 ml) and conc. hydrochloric acid (1.04 g) were added to the resulting residue (E/Z=41/59), and the mixture was stirred at room temperature for 20.5 hours. After completion of the reaction, water (300 ml) was added. The mixture was extracted with ethyl acetate (300 ml), washed with brine twice, dried over anhydrous magnesium sulfate and concentrated under reduced pressure to give (E)-N-methyl-2-(2-phenoxyphenyl)-2-hydroxyiminoacetamide (2.58 g, Yield: 95.6%, E/Z=96/4).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05442063 |
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| 出典データセット | uspto-grants-1995_08 |
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| ORD ID | ord-7c9cf26173fc4b8faa042d219230fcd1 |
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| 出典メモ | uspto-grants-1995_08 |
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