関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Acrylamide | HCID 6579 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | N-acetyl methacrylamide | HCID 21867965 | 4% |
反応手順
23.7 g of acrylamide and 60 ml of triethylamine were dissolved in 100 ml of dichloromethane in a flask. To the solution was then added dropwise 27.6 g of acetyl chloride at a temperature of −30° C. After the termination of the dropwise addition, the mixture was then stirred at a temperature of 0° C. for 10 hours. Triethylamine hydrochloride thus precipitated was then filtered off. The filtrate was then subjected to distillation under reduced pressure to remove the solvent therefrom. The residue thus obtained was then subjected to column chromatography with ethyl acetate as a developing solvent and silica gel as a filler to obtain 1.5 g of the desired compound (yield: 4%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07732550B2 |
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| 出典データセット | uspto-grants-2010_06 |
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| ORD ID | ord-1ae4c6ad69704a90874bb03b4ccd8ab6 |
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| 出典メモ | uspto-grants-2010_06 |
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