関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 2-chloro-N-(2,4-dimethoxyphenyl)acetamide | HCID 303824 | — |
| 反応物 | Aluminum(III) Chloride | HCID 6451240 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Chloroacetamido-5-methoxy phenol | HCID 13506553 | 92% |
反応手順
2-Chloro-N-(2,4-dimethoxy-phenyl)-acetamide (45.8 g, 0.2 mol) was dissolved in 1000 mL methylene chloride, and the reaction mixture was stirred at 0° C. under nitrogen. Aluminum trichloride (78.9 g, 0.6 mol) was added in portions over 30 minutes, and the reaction mixture was allowed to stir for 17 hours at room temperature. The reaction mixture was concentrated to 200 mL volume under reduced pressure, and then poured onto ice. Solids were removed by filtration, and the liquid was taken up in EtOAc, washed with brine, dried (MgSO4), filtered, and evaporated under reduced pressure to yield 39.67 g of 2-Chloro-N-(2-hydroxy-4-methoxy-phenyl)-acetamide. MS (M+H)=216.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524725B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-1df77548902c412289a0d4218c428ab1 |
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| 出典メモ | uspto-grants-2013_09 |
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