関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Methylamine | HCID 6329 | — |
| 反応物 | methyl (2E)-2-hydroxyimino-2-(2-phenoxyphenyl)acetate | HCID 88276687 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (E)-2-(Hydroxyimino)-N-methyl-2-(2-phenoxyphenyl)acetamide | HCID 9816878 | 61% |
反応手順
To crude E-a-hydroxyimino-2-phenoxyphenylacetic acid methyl ester (39.6 g, 0.0747 mole, purity: 51.2%) were added methanol (100 ml) and 40% aqueous solution of methylamine (15.45 g, 0.199 mole) and the mixture was stirred at room temperature for 15 hours. Then, 40% aqueous solution of methylamine (7.73 g, 0.0995 mole) was added to the mixture which was stirred in an oil bath at 70° C. for 6 hours. After completion of the reaction, water (200 ml) and toluene (100 ml) were added to the reaction mixture, which was stirred with ice cooling for one hour. The precipitated crystals were filtered off and recrystallized (methanol/toluene) to obtain E-2-hydroxyimino-N-methyl-2-(2-phenoxyphenyl)acetamide (12.31 g, yield: 60.1%) as colorless crystals (melting point: 183°-184.5° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05488159 |
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| 出典データセット | uspto-grants-1996_01 |
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| ORD ID | ord-96ca491ac0e4457f970b189090d63d42 |
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| 出典メモ | uspto-grants-1996_01 |
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