関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Bromophenol | HCID 7808 | — |
| 反応物 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | (2,3-Difluorophenyl)boronic acid | HCID 2734333 | — |
| 触媒 | HCID 178418397 | HCID 178418397 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 4-(2,3-Difluorophenyl)phenol | HCID 18920834 | 75% |
反応手順
First, 34.6 g of 4-bromphenol, 37.9 g of 2,3-difluorophenylboronic acid, 380 ml of dimethoxyethane, 380 ml of water, 97.8 g of cesium carbonate, and 7 g of tetrakis(triphenylphosphine)palladium were placed in a 1 L flask. The mixture was stirred under reflux for 20 hours. The reaction mixture was poured into water and an organic layer was extracted with ether. The ether layer was washed with water and dried over anhydrous sodium sulfate. Thereafter, the solvent was distilled away. The residue was purified by silica gel column chromatography (eluent: toluene/ethyl acetate=9/1) and recrvstallized from hexane to obtain 30.9 g of 2,3-difluoro-4'-hydroxybiphenyl (Y: 75%). The compound thus obtained had a purity of 99.8% by GC and an m.p. of 132° C. to 134.4° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05750213 |
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| 出典データセット | uspto-grants-1998_05 |
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| ORD ID | ord-7a826045604c4a2db7210bd703efeeed |
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| 出典メモ | uspto-grants-1998_05 |
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