関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chloroacetyl chloride | HCID 6577 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,4-Dimethoxyaniline | HCID 17652 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-chloro-N-(2,4-dimethoxyphenyl)acetamide | HCID 303824 | 99.2% |
反応手順
A mixture of 2,4-dimethoxy aniline (30.6 g, 0.2 mol), triethylamine (27.9 mL, 0.2 mol) in 600 mL methylene chloride was stirred at 0° C. under nitrogen. Chloroacetyl chloride (16 mL, 0.2 mol) was added dropwise, and the reaction mixture was stirred for 15 minutes at 0° C., and then stirred for an additional two hours during which time the reaction mixture was allowed to warm to room temperature. The reaction was quenched by addition of 1N HCl, followed by saturated aqueous sodium bicarbonate. The aqueous mixture was partitioned with EtOAc, and the organic phase was separated, dried (MgSO4), filtered, and evaporated under reduced pressure to give 45.58 g of crude 2-Chloro-N-(2,4-dimethoxy-phenyl)-acetamide. MS (M+H)=230.
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-28c78f0b87814c96b80a9efd1ceacb5d |
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| 出典メモ | uspto-grants-2013_09 |
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