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2,3-Difluoroaniline → N-(2,3-difluorophenyl)-3-nitropyridin-4-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,3-Difluoroaniline | HCID 78278 | — |
| 反応物 | 4-Chloro-3-nitropyridine | HCID 2735781 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | N-(2,3-difluorophenyl)-3-nitropyridin-4-amine | HCID 58180163 | 79% |
反応手順
To a solution of 4-chloro-3-nitropyridine (3.0 g, 18.9 mmol) in dry ethanol as added 2,3-difluorobenzenamine (3.66 g, 28.3 mmol). The reaction mixture was refluxed for 30 min. After cooling and concentration in vacuo to give a brown solid, the crude product was taken up in water and the aqueous solution adjusted to a pH of 8-9 and the solution extracted with EtOAc (3×100 mL). The combined organics were washed with water (3×100 mL) and brine solution (1×100 mL), respectively, dried over Na2SO4, and evaporated in vacuo to give a light brown solid. The crude product was triturated with petroleum ether (3×30 mL) to afford N-(2,3-difluorophenyl)-3-nitropyridin-4-amine (3.7 g, 79% yield) as light yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07872031B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-e9358eacbac64b1db36466971a01d6c1 |
| 出典メモ | uspto-grants-2011_01 |