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Phosphorus oxychloride → 4-Chloro-3-methoxy-2-methylpyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 3-Methoxy-2-methyl-1H-pyridin-4-one | HCID 323424 | — |
| 生成物 | 4-Chloro-3-methoxy-2-methylpyridine | HCID 10583046 | — |
反応手順
3-Methoxy-2-methyl-4(1H)-pyridone (5.6 g) was suspended in phosphorus oxychloride (50 ml), refluxed for 10 hours, and concentrated. To the resultant residue was added toluene and the residual phosphorus oxychloride was evaporated under reduced pressure. To the resultant oily substance were added chloroform and water and the chloroform layer was separated. The aqueous layer was made alkaline with potassium carbonate and extracted with chloroform. The chloroform solutions thus obtained were combined, washed with water, dried, and evaporated. The residue was purified by column chromatography on silica gel, to give 4-chloro-3-methoxy-2-methylpyridine (4.8 g) as a light brown oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04738975 |
| 出典データセット | uspto-grants-1988_04 |
| ORD ID | ord-f14632ad3c684d5caf7fc9c6037bd456 |
| 出典メモ | uspto-grants-1988_04 |