関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Catechol | HCID 289 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 2',3'-Dihydroxyacetophenone | HCID 6429110 | — |
反応手順
In the solution of 220 g(2 mol) of catechol in 500 ml of acetic acid, 102 g(1 mol) of acetic anhydride was drop-added for one hour while agitating the solution at 110° C. The mixture was maintained at 110° C. for two hours, and diethylene glycol dibutyl ether was distilled under vacuum. 1 Liter of toluene was added to the reaction mixture and cooled to 0° C. and then the unreacted excess hydroquinone was filtered and collected (recovered amount: 110 g, recycled without any purification process). A desired mono acetyl catechol was obtained by evaporating the residue in vacuum. (Yield: 149.0 g(98%). mp: oil. 1H-NMR(200 MHz, CDCl3, ppm) 2.33(s, 3H), 5.81 (br, 1H), 6.83-7.18 (m, 4H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06933403B2 |
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| 出典データセット | uspto-grants-2005_08 |
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| ORD ID | ord-740d69d6ac5944849707f997383b156d |
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| 出典メモ | uspto-grants-2005_08 |
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