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Hydrochloric Acid → N-(3-fluoro-4-methylphenyl)-3-nitro-2-pyridylamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Water | HCID 962 | — |
| 反応物 | 3-Fluoro-4-methylaniline | HCID 9957 | — |
| 反応物 | 2-Chloro-3-nitropyridine | HCID 79613 | — |
| 溶媒 | Glycol monoethyl ether | HCID 8076 | — |
| 生成物 | N-(3-fluoro-4-methylphenyl)-3-nitro-2-pyridylamine | HCID 40676958 | 82,342.5% |
反応手順
45 g (0.28 mmol) of 2-chloro-3-nitropyridine was dissolved in 2-ethoxyethanol (300 ml), and 36 g (0.28 mmol) of 3-fluoro-4-methylaniline, 12N-hydrochloric acid and water (300 ml) were added thereto. Mixed solution was heated to reflux for 24 hours while stirring. The reaction solution was cooled to room temperature, and the solvent was distilled off under reduced pressure. The solution was extracted with ethyl acetate, and washed with saturated brine, and then the obtained organic layer was dried over anhydrous magnesium sulfate. The mixture was concentrated under reduced pressure, and the residue thus obtained was washed with diisopropyl ether to obtain 57 g (yield: 82%) of N-(3-fluoro-4-methylphenyl)-3-nitro-2-pyridylamine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08648075B2 |
| 出典データセット | uspto-grants-2014_02 |
| ORD ID | ord-9fbcc228a5194e8cae52bfc3ab30a05f |
| 出典メモ | uspto-grants-2014_02 |