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HRID 1692614作成日:2026年10月26日
2,6-Dibromo-3,5-dihydroxy-4[(dimethylamino) methylene]-benzoic Acid → 3,5-Dihydroxy-4-methylbenzoic Acid
https://huagongshe.com/reaction/1692614
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
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| 反応物 | 2,6-Dibromo-3,5-dihydroxy-4[(dimethylamino) methylene]-benzoic Acid | HCID 86643250 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 3,5-Dihydroxy-4-methylbenzoic Acid | HCID 2748045 | 70% |
反応手順
To a stirred solution of 2,6-Dibromo-3,5-dihydroxy-4[(dimethylamino) methylene]-benzoic Acid (1 mmol) in 2.5 mL of 3 N NaOH under nitrogen was added 0.345 g of Raney nickel in portions over a period of 1 h. The mixture was then stirred at 25° C. for about 12 h and filtered. The filter cake was washed with water (2×5 mL), and the combined filtrates were acidified to a pH of 1 with concentrated HCl to give a pale yellow or light purple solution. The solution was extracted with ethyl acetate, and the combined organic extracts were washed with saturated NaCl solution (2×0.2 mL), dried over sodium sulphate and evaporated by a rotatory evaporator to give 3,5-Dihydroxy-4-methylbenzoic Acid (70%) as a white solid: 1H NMR (DMSO-d6) δ 6.90 (s, 2H), 1.95 (s, 3H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08158623B2 |
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| 出典データセット | uspto-grants-2012_04 |
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| ORD ID | ord-a21c5f64929b4c32b1396deb9ccc317f |
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| 出典メモ | uspto-grants-2012_04 |
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