関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethylene Glycol | HCID 174 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 2-Methyl-4-(trifluoromethyl)benzonitrile | HCID 22250332 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Methyl-4-(trifluoromethyl)benzoic acid | HCID 22211658 | — |
反応手順
Potassium hydroxide (15.7 g, 0.28 mole) and 15 mL of water were added as a solution to a stirred, heterogeneous mixture of 2-methyl-4-(trifluoromethyl)benzonitrile (13 g, 70 mmol) and 135 mL of ethylene glycol. The reaction mixture was heated at 120-130° C. for 20 hours and allowed to cool to room temperature. The dark solution was poured into 800 mL of water and filtered through celite. The filtrate was washed with ether and then the aqueous was acidified with concentrated hydrochloric acid. This aqueous phase was extracted three times with ethyl acetate, the organic extracts were combined, dried over magnesium sulfate and evaporated under reduced pressure to afford the title compound as a tan solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06747047B2 |
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| 出典データセット | uspto-grants-2004_06 |
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| ORD ID | ord-6e1b9d0593fe47309ae70c5aa6df543d |
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| 出典メモ | uspto-grants-2004_06 |
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