関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-(3-fluoro-4-nitrophenyl)-1H-1,2,4-triazole | HCID 21883919 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-Fluoro-4-(1,2,4-triazol-1-yl)phenylamine | HCID 21883866 | 64.1% |
反応手順
1-(3-Fluoro-4-nitrophenyl)-1H-1,2,4-triazole (3.06 g) was dissolved in ethanol (100 ml) and admixed with 10% Pd/C (50% water, 612 mg) and then stirred under a hydrogen atmosphere at room temperature for 1 hour. After filtering the catalyst off, the filtrate was concentrated under reduced pressure. The residue was diluted with ethyl acetate, and the resultant solution as washed successively with water and saturated brine, and dried over magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was purified by column chromatography on silica gel (ethyl acetate/hexane=1:2). A desired fraction was concentrated under reduced pressure and the residue was crystallized from a mixture of ethyl acetate and diisopropyl ether to yield 1-(4-amino-3-fluorophenyl)-1H-1,2,4-triazole (1.68 g) as yellow powdery crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06495604B1 |
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| 出典データセット | uspto-grants-2002_12 |
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| ORD ID | ord-b70b8a07105d416b8fe25803d4567585 |
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| 出典メモ | uspto-grants-2002_12 |
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