関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 2-Fluoro-4-(trifluoromethyl)benzaldehyde | HCID 522929 | — |
| 反応物 | HCID 178418816 | HCID 178418816 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-[2-Fluoro-4-(trifluoromethyl)phenyl]-3-methylbutanol | HCID 66883444 | 23% |
反応手順
To mixed solution of 2M isobutylmagnesium bromide in THF (6.25 mL) and ether (50 mL), was added dropwise a solution of 2-fluoro-4-(trifluoromethyl)benzaldehyde (2.0 g, 10 mmol) in ether (18 mL) under N2 atmosphere. The mixture was stirred at room temperature for 45 minutes, to which was added saturated aqueous ammonium chloride solution and 1M hydrochloric acid under ice-cooling. The aqueous layer was extracted with ether. The organic layer was washed with saturated aqueous sodium bicarbonate solution, saturated brine successively. After drying over anhydrous sodium sulfate, the solvent was removed under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate=10/1), to give the titled compound as a yellow oil (601 mg, yield 23%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08648208B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-f19fe8998cd942088cff0df91f4902de |
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| 出典メモ | uspto-grants-2014_02 |
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