関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1-Chloro-3-iodobenzene | HCID 12269 | — |
| 反応物 | Benzene, 1,3-dichloro-2-fluoro-5-(trifluoromethyl)- | HCID 157026 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 溶媒 | Butyllithium | HCID 178418339 | — |
| 生成物 | 1-Chloro-3-(2,6-dichloro-4-trifluoromethylphenyl)benzene | HCID 22170926 | 36.7% |
反応手順
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%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06858639B2 |
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| 出典データセット | uspto-grants-2005_02 |
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| ORD ID | ord-f2cfb412bf3d4b57a1c11a5247038448 |
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| 出典メモ | uspto-grants-2005_02 |
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