참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Carbon Dioxide | HCID 280 | — |
| 반응물 | Diisopropylamine | HCID 7912 | — |
| 반응물 | 1-Bromo-2,3,4-trifluorobenzene | HCID 2733255 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 5-Bromo-2,3,4-trifluorobenzoic acid | HCID 11118637 | 88% |
반응 단계
To a solution of iPr2NH (56.8 mmol, 8 ml) in THF (50 ml) at −78° C. was added dropwise a solution of nBuLi (1.6M in hexane, 56.8 ml, 35.5 mmol). The dry ice bath was removed and the mixture was stirred at 0° C. for ˜15 min. The mixture is transferred via cannula to a solution of 1-bromo-2,3,4-trifluorobenzene (47.4 mmol, 10 g) in THF (50 ml) cooled at −78° C. The orange solution was stirred at −78° C. for 1 h, then transferred, via cannula, to freshly grinded dry CO2. The reaction was warmed up to room temperature and stirred overnight. The reaction mixture was cooled at 0° C., quenched with 10% HCl (300 ml), extracted with ether (100 ml×3), dry over MgSO4 and concentrated under reduced pressure to obtain (10.6 g, 88%) of the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08063049B2 |
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| 출처 데이터셋 | uspto-grants-2011_11 |
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| ORD ID | ord-d6a4fcbb976440079bb1606a45ae0388 |
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| 출처 메모 | uspto-grants-2011_11 |
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