참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | 1-Chloro-3-iodobenzene | HCID 12269 | — |
| 반응물 | Benzene, 1,3-dichloro-2-fluoro-5-(trifluoromethyl)- | HCID 157026 | — |
| 용매 | Benzene | HCID 241 | — |
| 용매 | Hexane | HCID 8058 | — |
| 용매 | Butyllithium | HCID 178418339 | — |
| 생성물 | 1-Chloro-3-(2,6-dichloro-4-trifluoromethylphenyl)benzene | HCID 22170926 | 36.7% |
반응 단계
To 10.0 g (41.9 mmol) of 1-chloro-3-iodobenzene in 50 ml of dry benzene, 32.0 ml of a n-butyllithium solution in hexane (1.56 mol/l) was added dropwise in a nitrogen stream at room temperature with stirring. After another 2 hours of stirring at room temperature, 9.9 g (42.5 mmol) of 3,5-dichloro-4-fluorobenzotrifluoride was added dropwise at 10° C. After another 12 hours of stirring at room temperature, the reaction mixture was poured into 500 ml of water for separation. The organic layer was washed with 200 ml of water twice and dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. Purification of the residue by silica gel column chromatography afforded 5.0 g of 1-chloro-3-(2,6-dichloro-4-trifluoromethylphenyl)benzene (yield 35.0%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06858639B2 |
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| 출처 데이터셋 | uspto-grants-2005_02 |
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| ORD ID | ord-f2cfb412bf3d4b57a1c11a5247038448 |
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| 출처 메모 | uspto-grants-2005_02 |
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