関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Iodoethane | HCID 6340 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2-Hydroxy-4-(trifluoromethyl)benzoic acid | HCID 164578 | — |
| 生成物 | Ethyl 2-ethoxy-4-(trifluoromethyl)benzoate | HCID 66857656 | 74% |
反応手順
To a solution of 2-hydroxy-4-trifluoromethyl-benzoic acid (5 g, 24.258 mmol, Matrix Scientific) in ethanol (50 mL) were added potassium carbonate (8.38 g, 60.645 mmol) and ethyl iodide (7.68 mL, 97.032 mmol). The reaction mixture was heated at gentle reflux for 4 h then concentrated in vacuo. The residue was taken in petroleum ether and water, and the layers were separated. The product was extracted with petroleum ether (1×). The organic layers were washed with brine (1×), dried over anhydrous sodium sulfate, filtered and concentrated. Purification of the crude residue by flash chromatography (40 g of silica gel, eluting with 10% ethyl acetate in hexane) gave 2-ethoxy-4-trifluoromethyl-benzoic acid ethyl ester as colorless oil (4.68 g, 74%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07851626B2 |
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| 出典データセット | uspto-grants-2010_12 |
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| ORD ID | ord-ffcb9308274d4c01b5ea162c5ded78cb |
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| 出典メモ | uspto-grants-2010_12 |
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