関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | (E)-2-(Hydroxyimino)-N-methyl-2-(2-phenoxyphenyl)acetamide | HCID 9816878 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | (2E)-2-methoxyimino-N-methyl-2-(2-phenoxyphenyl)acetamide | HCID 5483872 | 94.4% |
反応手順
To E-2-hydroxyimino-N-methyl-2-(2-phenoxyphenyl)acetamide (10.00 g, 0.037 mole) were added acetone (200 ml), potassium carbonate (15.34 g, 0.111 moles) and dimethylsulfate (9.33 g, 0.074 moles) and the mixture was stirred at room temperature for 9 hours. After completion of the reaction, the reaction mixture was filtered, washed with acetone and concentrated under reduced pressure. The oil thus obtained was dissolved in toluene (50 ml) and to this was added an aqueous 1N sodium hydroxide solution (50 ml), followed by stirring at room temperature for 30 minutes. The mixture was extracted with toluene, washed with water and concentrated, and then the resulting residue was recrystallized (methanol/water) to obtain E-2-methoxyimino-N-methyl-2-(2-phenoxyphenyl)acetamide (9.93 g, yield: 94.4%) as colorless crystals (melting point: 81.5°-83° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05650539 |
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| 出典データセット | uspto-grants-1997_07 |
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| ORD ID | ord-348df9e600d44c64a47a017bf5c79b35 |
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| 出典メモ | uspto-grants-1997_07 |
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