関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 3'-Fluoro-4'-methoxy-4-acetylbiphenyl | HCID 14388648 | — |
| 反応物 | Sodium Bisulfite | HCID 23665763 | — |
| 反応物 | Sodium hypobromite | HCID 23673712 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 3'-Fluoro-4'-methoxy-[1,1'-biphenyl]-4-carboxylic acid | HCID 1203166 | 94% |
反応手順
The resulting 4-acetyl-3'-fluoro-4'-methoxybiphenyl (7.2 g) was dissolved in 300 ml of dioxane, and 360 ml of a solution of sodium hypobromite (prepared from 75 g of sodium hydroxide and 78 g of bromine) was added over about 40 minutes at 0° to 5° C., and the mixture was stirred at 30° to 35° C. for 2 hours. The excess of sodium hypobromite was decomposed with a saturated aqueous solution of sodium hydrogen sulfite, and 10% hydrochloric acid was added to adjust the pH of the solution to 3 to 4. The solution was left to stand at 10° C. for 20 hours to permit crystallization. The resulting crystals were filtered to give 7.2 g of 3'-fluoro-4'-methoxybiphenyl-4-carboxylic acid. Recrystallization from isopropyl alcohol gave 6.8 g of the desired product. Yield 94%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04914224 |
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| 出典データセット | uspto-grants-1990_04 |
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| ORD ID | ord-1b36cf96598f485bbcb64926a71422ec |
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| 出典メモ | uspto-grants-1990_04 |
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