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Hydrochloric Acid → 2-Amino-5-chloropyridin-3-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 3,5-Dichloro-3-pyridylamine | HCID 77886 | — |
| 触媒 | Copper | HCID 23978 | — |
| 溶媒 | Diglyme | HCID 8150 | — |
| 生成物 | 2-Amino-5-chloropyridin-3-ol | HCID 10313200 | 70% |
反応手順
A mixture of 20 parts of 2-amino-3,5-dichloropyridine, 160 parts of glycol, 80 parts of potassium hydroxide, 1 part of copper powder and 3 parts of diethylene glycol dimethyl ether is stirred under nitrogen for 5 hours at 150°-160° C. The cooled solution is neutralised with conc. hydrochloric acid, saturated with sodium chloride and extracted twice in the warm state with ethyl acetate. The combined extracts are filtered through Hyflo, dried over magnesium sulphate and purified with active charcoal. The solvent is evaporated off to leave 12.3 parts (70% of theory) of 2-amino-3-hydroxy-5-chloropyridine, m.p. 198°-201° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04033975 |
| 出典データセット | uspto-grants-1977_07 |
| ORD ID | ord-7b568c3df9f444d6a72ba2742e3cce12 |
| 出典メモ | uspto-grants-1977_07 |