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Acetic Acid → 2-Amino-4,6-dimethylbenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 4,6-dimethyl-1H-indole-2,3-dione | HCID 2386161 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 2-Amino-4,6-dimethylbenzoic acid | HCID 13380623 | — |
反応手順
To a heated (70° C. bath temperature) deep red solution of 4,6-dimethyl-1H-indole-2,3-dione (1.00 g, 5.71 mmol) in 33% aqueous sodium hydroxide (35 mL) was added 35% hydrogen peroxide (3.33 g, 34.3 mmol) over a period of 5 minutes. The reaction mixture was heated for another 15 min, then cooled to room temperature, and ice was added. The pH was adjusted to approximately 8 with concentrated HCl at 0° C. and acidified further to pH approximately 6 with glacial acetic acid. The solid precipitated was filtered, washed well with cold water, and dried under vacuum at 40° C. overnight to obtain 2-amino-4,6-dimethyl-benzoic acid as a pale brown solid. Yield: 0.35 g (37%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09238640B2 |
| 出典データセット | uspto-grants-2016_01 |
| ORD ID | ord-a507092f3d674698885eda1e829ff638 |
| 出典メモ | uspto-grants-2016_01 |