関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Hydrogen Peroxide | HCID 784 | — |
| 反応物 | 2-Methyl-5-hydroxypyridine | HCID 14275 | — |
| 生成物 | 2-Chloro-6-methylpyridin-3-ol | HCID 3015797 | — |
反応手順
In 500 ml conc. hydrochloric acid was dissolved 50.0 g (0.46 mole) 6-methyl-3-hydroxypyridine. After heating to 80° C., 150 ml 15% hydrogen peroxide was slowly added over several hours while maintaining the reaction temperature at 80°-85°. The reaction mixture was cooled to 50° C. and concentrated under reduced pressure. The residue was brought to pH 8 by careful addition of 25% sodium hydroxide solution. This mixture was extracted with ether. The solvent was removed and the residue recrystallized one time from water and one time from benzene to provide pure 2-chloro-6-methyl-3-hydroxypyridine, mp 190°-191° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04220577 |
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| 出典データセット | uspto-grants-1980_09 |
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| ORD ID | ord-1a543677da5144988b7c4bf06f929195 |
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| 出典メモ | uspto-grants-1980_09 |
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