化工社化工社 化学情報印刷レポート · 研究参考用
Water → 1-Fluoro-2-trifluoromethoxy-6-[(4-propylphenyl)ethynyl]naphthalene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Toluene | HCID 1140 | — |
| 反応物 | 1-Ethynyl-4-propylbenzene | HCID 2775133 | — |
| 反応物 | 2-Bromo-5-fluoro-6-trifluoromethoxynaphthalene | HCID 21870154 | — |
| 触媒 | Copper iodide | HCID 83717 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Fluoro-2-trifluoromethoxy-6-[(4-propylphenyl)ethynyl]naphthalene | HCID 21869758 | 36.6% |
反応手順
10 g of 4-propyl-1-ethynylbenzene and 19.5 g of 2-bromo-5-fluoro-6-trifluoromethoxynaphthalene were dissolved in 50 ml of N,N-dimethylformamide (DMF). To the solution were then added 50 mg of copper iodide (I) and 100 mg of tetrakis(triphenylphosphine)palladium (0). The reaction mixture was then stirred at room temperature for 5 hours. To the reaction solution was then added toluene. Insoluble matters water removed by filtration. The residue was then washed with water and saturated brine. The solvent was then distilled off. The residue was purified through silica gel column chromatography (hexane/ethyl acetate 9/1), and then recrystallized from ethanol to obtain 8.6 g of 1-fluoro-2-trifluoromethoxy-6-[(4-propylphenyl)ethynyl]naphthalene.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07145047B2 |
| 出典データセット | uspto-grants-2006_12 |
| ORD ID | ord-ef3929760d114f2eb3d9bca52eaacad3 |
| 出典メモ | uspto-grants-2006_12 |