化工社化工社 化学情報印刷レポート · 研究参考用
Water → 4-(2,6-Dichloro-4-trifluoromethylphenyl)toluene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Iodotoluene | HCID 12207 | — |
| 反応物 | Benzene, 1,3-dichloro-2-fluoro-5-(trifluoromethyl)- | HCID 157026 | — |
| 溶媒 | Benzene | HCID 241 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 溶媒 | Hexane | HCID 8058 | — |
| 溶媒 | Butyllithium | HCID 178418339 | — |
| 生成物 | 4-(2,6-Dichloro-4-trifluoromethylphenyl)toluene | HCID 22170961 | 85.1% |
反応手順
To 5.7 g (26.1 mmol) of 4-iodotoluene in 30 ml of dry benzene, 17.0 ml of a n-butyllithium solution in hexane (1.60 mol/l) was added dropwise in a nitrogen stream at room temperature with stirring. After 2 hours of stirring at room temperature, 10 ml of 6.0 g (25.8 mmol) of 3,5-dichloro-4-fluorobenzotrifluoride in 10 ml of diethyl ether was added dropwise at 10° C. After another 12 hours of stirring at room temperature, the reaction mixture was poured into 100 ml of water for separation. The organic layer was washed with 50 ml of water twice and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 6.7 g of 4-(2,6-dichloro-4-trifluoromethylphenyl)toluene (yield 85.0%) as a colorless liquid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07612105B2 |
| 出典データセット | uspto-grants-2009_11 |
| ORD ID | ord-b33c75a50a9e45cfb1521f3712331de9 |
| 出典メモ | uspto-grants-2009_11 |