참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | 2-Fluoro-4-(trifluoromethyl)benzaldehyde | HCID 522929 | — |
| 반응물 | HCID 178418816 | HCID 178418816 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-[2-Fluoro-4-(trifluoromethyl)phenyl]-3-methylbutanol | HCID 66883444 | 23% |
반응 단계
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%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08648208B2 |
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| 출처 데이터셋 | uspto-grants-2014_02 |
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| ORD ID | ord-f19fe8998cd942088cff0df91f4902de |
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| 출처 메모 | uspto-grants-2014_02 |
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