関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-(4'-Fluoro(1,1'-biphenyl)-4-yl)ethanone | HCID 608114 | — |
| 反応物 | Sodium Pyrosulfite | HCID 656671 | — |
| 反応物 | Acetic acid;1,1'-biphenyl | HCID 21957439 | — |
| 反応物 | sodium hypobromite | HCID 178507097 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 4-(4-Fluorophenyl)benzoic acid | HCID 2782689 | — |
反応手順
NaOH (7 g) was dissolved in water (25 mL) and cooled in an ice bath. Bromine (7.8 g) was added dropwise to give a solution of NaOBr. 1-(4′-Fluoro-biphenyl-4-yl)-ethanone (0.01 mol) was dissolved in dioxane (35 mL) and warmed to 50° C. in a water bath. The NaOBr solution was added slowly to the stirred solution of the biphenyl acetate and stirring continued at 50° C. for a further 20 minutes. The solution was allowed to cool and a solution of sodium metabisulphite (8 g in 40 mL water) was added followed by water (170 mL). 50 mL of the liquid was evaporated under reduced pressure with heating. The remainder was acidified with HCl (5 mL) and a white precipitate formed upon cooling. The precipitate was filtered and recrystallised from acetic acid to give the title compound. δC (CDCl3, 62.9 MHz): 115.9, 126.8, 129.2, 129.6, 129.8 (d, J 2.9), 135.5 (d, J 2.9), 143.2, 162.4 (d, J 245.1) and 167.2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07598289B2 |
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| 出典データセット | uspto-grants-2009_10 |
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| ORD ID | ord-77c2e4ce4b68472d8f9e6655e4baedc1 |
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| 出典メモ | uspto-grants-2009_10 |
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