関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 3-Piperidinopropiophenone hydrochloride | HCID 70171 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 触媒 | Silver | HCID 23954 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | beta-Piperidinopropiophenone oxime | HCID 23906289 | 74.8% |
反応手順
In 470 ml of water were dissolved 60.2 g of β-piperidinopropiophenone hydrochloride and 18.1 g of hydroxylamine hydrochloride. To this solution was added portionwise 21.9 g of sodium hydrogencarbonate. After the whole amount was added, the mixture was stirred overnight. To the stirred mixture was then added an aqueous solution of 14.2 g of sodium hydroxide in 47 ml of water. Thus obtained mixture was well stirred and allowed to stand for 2 hours to produce a white precipitate. The precipitate was collected by filtration and washed successively with two portions of 200 ml of water and ethanol. The washed precipitate was dried to obtain a white solid. The solid was then recrystallized from methanol to obtain 41.2 g (yield: 74.8%) of the subject compound as a silver-white scaly product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04764617 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-e9c738adc29e404d9db764e041f0902d |
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| 出典メモ | uspto-grants-1988_08 |
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