関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | 1-(2,6-Difluorophenyl)ethan-1-one | HCID 83643 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(2,6-Difluoro-3-nitrophenyl)ethanone | HCID 13853637 | — |
反応手順
To a −40° C. mixture of concentrated H2SO4 (100 mL) and fuming HNO3 (100 mL) was added 1-(2,6-difluorophenyl)ethanone (20 g, 128 mmol) dropwise. The resulting mixture was stirred at −40° C. for 2 h then poured slowly onto ice. That mixture was diluted with DCM and the phases were separated. The aqueous layer was neutralized with sat. aq. NaHCO3 and then extracted with DCM. All organic portions were combined, dried over MgSO4, filtered, and concentrated to give 1-(2,6-difluoro-3-nitrophenyl)ethanone (26.3 g, 131 mmol, >theoretical) that was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09029362B2 |
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| 出典データセット | uspto-grants-2015_05 |
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| ORD ID | ord-fdffe23e2db44304b83f1530697be30a |
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| 出典メモ | uspto-grants-2015_05 |
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