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Ethanol → 2-(Acetylamino)-3-(3,4-dimethylphenyl)propanoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | Diethyl 2-acetylamino-2-(3,4-dimethylbenzyl)malonate | HCID 13406779 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(Acetylamino)-3-(3,4-dimethylphenyl)propanoic acid | HCID 2747249 | 56% |
反応手順
Diethyl 2-acetylamino-2-(3,4-dimethylbenzyl)malonate (13.8 g) and potassium hydroxide (2.76 g) were dissolved into a mixed solution of ethanol (138 ml) and water (138 ml) and the solution was stirred under reflux for 8.5 hours. After being cooled to room temperature, the solution was concentrated under reduced pressure and the resulting aqueous solution was adjusted to pH 10 with aqeuous saturated sodium hydrogen carbonate solution. The solution was washed with ethyl acetate and made acidic with diluted hydrochloric acid, and extracted with ethyl acetate. The extract was dried over magnesium sulfate and evaporated under reduced pressure to give crystals of N-acetyl-3,4-dimethyl-DL-phenylalanine (5.42 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06924278B2 |
| 出典データセット | uspto-grants-2005_08 |
| ORD ID | ord-cfecf31e74744b2c93c7ed4c8d823992 |
| 出典メモ | uspto-grants-2005_08 |