関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Catechol | HCID 289 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 2,4-Difluoronitrobenzene | HCID 67967 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 溶媒 | Sodium chloride; water | HCID 57417360 | — |
| 生成物 | o-(5-Fluoro-2-nitrophenoxy)phenol | HCID 19932387 | 55% |
反応手順
Catechol (103.8 g, 0.94 mol) and potassium carbonate (129.9 g, 0.94 mol) are added to a solution of 2,4-difluoronitrobenzene (50.0 g, 0.314 mol) in acetonitrile. The reaction mixture is stirred at 28° C. for 24 hours, poured into brine and extracted with ether. The organic extract is washed with brine, dried over anhydrous sodium sulfate and concentrated in vacuo to obtain a brown gum. Flash chromatography of the gum using silica gel and a 10% hexanes in methylene chloride solution gives the title product as a yellow solid (43 g) which is identified by 1HNMR spectral analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05424280 |
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| 出典データセット | uspto-grants-1995_06 |
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| ORD ID | ord-3ac0287e59ea458f9d86f75740575bec |
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| 出典メモ | uspto-grants-1995_06 |
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