関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2,4,5-Trichloroaniline | HCID 12487 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ethyl 2-oxocyclohexanecarboxylate | HCID 95543 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Oxocyclohexanecarboxylic acid | HCID 9942171 | — |
反応手順
To a solution of 2,4,5-trichloroaniline (2.48 g, 12.6 mmol) in H2O (5 mL), cooled to 0° C., conc. HCl (7.5 mL) was added, and then stirred for 20 min. NaNO2 (0.87 g, 12.0 mmol) dissolved in water (5 mL), was added slowly and the reaction was continued at 0° C. for 1 h, filtered and the filtrate was used further. In another setup, ethyl 2-oxocyclohexanecarboxylate (2.0 g, 12.0 mmol) was added to 5N NaOH (0.56 g) and stirred for 16 h. The reaction mixture was cooled to 0° C., conc. HCl (1.2 mL) was added slowly, stirred for another 45 min. to obtain 2-oxocyclohexanecarboxylic acid which was added to the filtrate (prepared above) at 0° C. The resulting yellow solid precipitate was filtered, air dried to give the title compound (1.7 g, 44%) which was used in the next step without any spectroscopic analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08987319B2 |
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| 出典データセット | uspto-grants-2015_03 |
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| ORD ID | ord-abdaac3e628b4d67a4222c8d68300ce8 |
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| 出典メモ | uspto-grants-2015_03 |
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