関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 2-Fluoro-6-(trifluoromethyl)benzoic acid | HCID 688123 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 6-Fluoro-3-nitro-2-trifluoromethyl-benzoic acid | HCID 21477352 | — |
反応手順
1.05 ml (23.3 mmol) of concentrated nitric acid (65%), which also was precooled to 0° C., is instilled in a solution of 17.5 ml of concentrated sulfuric acid and 2.5 g (12.0 mmol) of 2-fluoro-6-trifluoromethyl-benzoic acid, cooled to 0° C. It is allowed to stir for one more hour at 0° C. and then overnight at room temperature. It is then poured in a mixture of ice, water and dichloromethane, the organic phase is separated and the aqueous phase is extracted with dichloromethane. The organic solutions are combined, washed with saturated sodium chloride solution, dried on sodium sulfate and evaporated to dryness in a vacuum. The title compound is obtained in crystalline form.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05686492 |
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| 出典データセット | uspto-grants-1997_11 |
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| ORD ID | ord-62788c37a7ea49d1ad1694bc8f5df3e4 |
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| 出典メモ | uspto-grants-1997_11 |
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