참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Stannane, tributyl(1-ethoxyethenyl)- | HCID 619414 | — |
| 반응물 | 1-Bromo-3-(difluoromethyl)benzene | HCID 2769675 | — |
| 촉매 | HCID 178418476 | HCID 178418476 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 1-(3-(Difluoromethyl)phenyl)ethan-1-one | HCID 67510119 | 98% |
반응 단계
A mixture of 1-bromo-3-(difluoromethyl)benzene (0.72 g, 3.48 mmol), tributyl(1-ethoxyvinyl)tin (1.38 g, 3.83 mmol), dichlorobis(triphenylphosphine)-palladium(II) (0.24 g, 0.35 mmol) in toluene (12 mL) is heated at 100° C. under nitrogen atmosphere for 16 hours. After cooling to room temperature, 2M hydrochloric acid (12 mL) is added to the mixture. Then the resulting mixture is stirred at room temperature for 1 hour. The mixture is diluted with ethyl acetate (100 mL) and washed with water (100 mL). The organic layer is dried over sodium sulfate, and concentrated under reduced pressure. The residue is purified by column chromatography on silica-gel eluting with n-hexane/ethyl acetate (30:1) to give 0.58 g (98% yield) of the title compound as colorless oil.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09302991B2 |
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| 출처 데이터셋 | uspto-grants-2016_04 |
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| ORD ID | ord-7c6a5cf691324612944f048a01b81bdb |
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| 출처 메모 | uspto-grants-2016_04 |
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