関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 5-Bromonicotinamide | HCID 1808 | — |
| 溶媒 | Phosphorus oxychloride | HCID 24813 | — |
| 生成物 | 5-Bromonicotinonitrile | HCID 736793 | 70% |
反応手順
5-Bromo-3-pyridinylcarboxamide (10 g, 49.7 mmol) in phosphorus oxychloride (25 mL) was warmed to reflux for 18 h, allowed to cool to 25° C., concentrated in vacuo and carefully treated with satd. aqueous sodium bicarbonate (˜500 mL) until neutralized. The reaction mixture was diluted with CH2Cl2 (200 mL), stirred for 4 h, and the layers were separated. The aqueous layer was washed with CH2Cl2 (2×100 mL), and the organic layers were combined and dried (MgSO4). The resulting solution was concentrated in vacuo to afford the title compound (6.35 g, 70%) as a white solid. MS 184 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06713455B2 |
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| 出典データセット | uspto-grants-2004_03 |
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| ORD ID | ord-30c79bf012b64918808d4c344a0bd047 |
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| 出典メモ | uspto-grants-2004_03 |
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