関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Phosphorus oxybromide | HCID 24613 | — |
| 反応物 | 6-Phenyl-2-pyridone | HCID 87889 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Bromo-6-phenylpyridine | HCID 568679 | 76% |
反応手順
A mixture of 6-phenyl pyridone (3 g, 17.5 mmol; prepared according to Example 6) and phosphoryl bromide (7.2 g, 25.0 mmol) is heated to 100° C. for 5 h. The cooled mixture is poured into water (40 ml) and the pH is adjusted to 9 by addition of saturated aqueous sodium carbonate. Then the layers are separated and the aqueous layer is extracted with ethyl acetate (50 ml). The combined organic layers are dried with anhydrous magnesium sulphate and the solvent is evaporated in vacuo. The crude product is crystallized from aqueous ethanol. Subsequent purification by flash chromatography (silica gel, hexane/ethyl acetate 9/1 v/v) gives 2-bromo-6-phenyl pyridine (3.1 g, 76% of th.) as light brown crystals with mp 50° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06008161 |
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| 出典データセット | uspto-grants-1999_12 |
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| ORD ID | ord-35f85b64668d492f987465c0c41694d3 |
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| 出典メモ | uspto-grants-1999_12 |
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