関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 5-Chloro-2-methylaniline | HCID 7260 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | N-(5-Chloro-2-methylphenyl)acetamide | HCID 80000 | — |
反応手順
5-Chloro-2-methyl-phenylamine (50 g, 353.11 mmol) was dissolved in dry THF (500 mL) followed by addition of triethylamine (61.53 mL, 441.39 mmol) and the whole heated to 60° C. To the stirring solution at 60° C. was added dropwise a solution of acetic anhydride (50 ml, 529.66 mmol) in dry THF (100 mL) and the reaction was stirred at 60° C. overnight. Upon cooling, the reaction was diluted with H2O (500 mL), ethyl acetate (250 mL) and the layers separated. The organics were washed with H2O (250 mL), 1N HCl (250 mL), sat Na2CO3 (250 mL), brine (250 mL), dried (MgSO4) and concentrated to a solid (59.67 g, 324.97 mmol).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07101886B2 |
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| 出典データセット | uspto-grants-2006_09 |
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| ORD ID | ord-a8ed8df5827746f9acc16b6f99be2e3e |
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| 出典メモ | uspto-grants-2006_09 |
|---|