関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 3-Fluoro-2-nitropyridine | HCID 2762802 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | (2-Nitropyridin-3-yl)phenylamine | HCID 20184004 | 154.2% |
反応手順
A mixture of 3-fluoro-2-nitropyridine (1.07 g, 6.75 mmol), aniline (1.8 mL, 20.2 mmol) and Et3N (2.8 mL, 20.2 mmol) in DMF (10 mL) was stirred at 100° C. for 16 h under a nitrogen atmosphere. After cooling to RT, the volatiles were removed under reduced pressure. The resulting residue was partitioned between DCM and water. The aqueous phase was further extracted with DCM (×3) and the combined organic fractions dried (Na2SO4) and concentrated in vacuo. The resulting residue was purified by column chromatography (Si—PCC, gradient 0-4% MeOH in DCM) to afford the title compound as a red oil (2.24 g, quantitative). LCMS (Method C): RT 3.03 min [M+H]+ 216.2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08653089B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-8f761dc54c3a4619aa346344671b6aeb |
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| 出典メモ | uspto-grants-2014_02 |
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