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Hydrochloric Acid → 5-Fluoro-pyridine-2-carbaldehyde oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | 5-Fluoropyridine-2-carboxaldehyde | HCID 10351697 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-Fluoro-pyridine-2-carbaldehyde oxime | HCID 136387251 | 79% |
反応手順
To a solution of 5-fluoro-2-formylpyridine (5.0 g, 41 mmol) and hydroxylamine hydrochloride (3.06 g, 44 mmol) in ethanol (3.2 mL) and water (9.6 mL) was added ice (18.6 g). Then a solution of NaOH (4.0 g, 100 mmol) in water (4.6 mL) was added dropwise over 10 min keeping the temperature between −5° C. and 5° C. The reaction mixture was then stirred at room temperature for 30 min. Then HCl (4 N) was added to acidify the mixture and the resulting precipitate was filtered off and washed with water to afford the title compound (4.41 g, 79%) as a light brown solid. MS: m/e=141.0 [M+H]+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08877782B2 |
| 出典データセット | uspto-grants-2014_11 |
| ORD ID | ord-c4591f9e032c47609b04058928a480f6 |
| 出典メモ | uspto-grants-2014_11 |