化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Iodide → Benzene, 4-bromo-2-[(4,4-difluoro-3-buten-1-yl)oxy]-1-fluoro-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Phenol, 5-bromo-2-fluoro- | HCID 183421 | — |
| 反応物 | 4-Bromo-1,1-difluorobut-1-ene | HCID 2782240 | — |
| 触媒 | Trioctylmethylammonium chloride | HCID 21218 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Methyl Ethyl Ketone | HCID 6569 | — |
| 生成物 | Benzene, 4-bromo-2-[(4,4-difluoro-3-buten-1-yl)oxy]-1-fluoro- | HCID 59790300 | 63% |
反応手順
A mixture of 2-fluoro-5-bromophenol (2.40 g), potassium carbonate (2.31 m), Aliquat 336 (5 drops), sodium iodide (catalytic) and 4-bromo-1,1-difluoro-1-butene (1.79 mL) in methyl ethyl ketone was placed in a pressure vessel and heated in a 82° oil bath for 15 hours. The reaction mixture was cooled, diluted with dichloromethane, filtered and evaporated in vacuo. The resultant residue was purified by flash chromatography (silica gel, eluant: 2.5% ethyl acetate/hexane to afford 4-bromo-2-(4,4-difluorobut-3-enyloxy)-1-fluorobenzene, 2.23 g (63% yield), identified by NMR analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07423158B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-64e03f43ee504125a8fbde98ebe10950 |
| 出典メモ | uspto-grants-2008_09 |