関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Phenylpyridine | HCID 13886 | — |
| 反応物 | Sodium amide | HCID 24533 | — |
| 溶媒 | P-Xylene | HCID 7809 | — |
| 生成物 | 5-Phenyl-2-pyridinamine | HCID 105097 | 55.8% |
| 生成物 | 3-Phenylpyridin-2-amine | HCID 2762795 | — |
反応手順
2-amino-3-phenyl pyridine was prepared as follows: 3-phenyl pyridine (300 mg, 2 mmol) was dissolved in para-xylene (6 ml), and sodamide (84 mg, 2.1 mmol) was then added. The reaction mixture was heated to reflux temperature for 8 hours. The reaction mixture was cooled, poured onto ice/water (25 ml), and extracted with dichloromethane. The organic extracts were washed with water and brine, and dried over anhydrous sodium sulphate. The sodium sulphate was removed by filtration, and the filtrate was evaporated to dryness and recrystallized from a mixture of diethyl ether and petroleum ether to provide 2-amino-5-phenyl pyridine (95 mg). The mother liquors from the crystallization were evaporated to dryness and subjected to purification by column chromatography (silica), thereby eluting the solvent ethyl acetate:petroleum ether (30:70). The desired product, 2-amino-3-phenyl pyridine, was obtained as a fine yellow powder (15 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06977255B2 |
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| 出典データセット | uspto-grants-2005_12 |
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| ORD ID | ord-021f73f6743b4b9bafbd63144bd27a87 |
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| 出典メモ | uspto-grants-2005_12 |
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