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Sodium Carbonate → 4-(4-Pyridyl)-2-butanone oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 4-(Pyridin-4-yl)butan-2-one | HCID 12707223 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 4-(4-Pyridyl)-2-butanone oxime | HCID 76539650 | 90% |
反応手順
Next, water (12 ml) and tetrahydrofuran (1.2 ml) were added to 4-(4-pyridyl)-2-butanone (736 mg, 3.96 mmol), and the mixture was stirred at room temperature. Sodium carbonate (483 mg, 4.56 mmol) and hydroxylamine hydrochloride (358 mg, 5.15 mmol) were added to the mixture, the whole was stirred for 1.5 hours, and then ethyl acetate (50 ml) was added to the reaction mixture to dilute it. Sodium hydrogencarbonate was added thereto. After separation, the organic layer was washed with saturated brine (10 ml), dried over anhydrous sodium sulfate and concentrated under reduced pressure. Cyclohexane was added to the resulting crystals, and the crystals were filtered off to give 4-(4-pyridyl)-2-butanone oxime (584 mg, 90%) as pale yellow crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07741346B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-a2942a5370974c94897ea627c6c2929b |
| 出典メモ | uspto-grants-2010_06 |