関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Isovaleryl chloride | HCID 66054 | — |
| 反応物 | 2,6-Dimethoxy-4-methylaniline | HCID 12409090 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | N-(2,6-dimethoxy-4-methylphenyl)isovaleramide | HCID 18936492 | 92% |
反応手順
8.2 g of 2,6-dimethoxy-4-methylaniline are dissolved in 100 ml of diethyl ether at 0° C. under an inert atmosphere, 5.96 g of triethylamine are added to the reaction mixture and then 6.51 g of isovaleryl chloride are added dropwise, while maintaining the temperature at 0° C. The mixture is left at room temperature for 30 minutes and is then poured into 250 ml of water. The aqueous phase is extracted with ethyl acetate after separation by settling of the ethereal phase. The organic phases are combined and washed with water, then dried over anhydrous sodium sulphate and evaporated to dryness. The white crystals of N-(2,6-dimethoxy-4-methylphenyl)isovaleramide obtained are washed with diisopropyl ether; M.p.=139° C., Yield: 92%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05731340 |
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| 出典データセット | uspto-grants-1998_03 |
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| ORD ID | ord-008f672ce81f498d931758715cd6380b |
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| 出典メモ | uspto-grants-1998_03 |
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