関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 1-Benzyl-4-cyano-4-phenylpiperidine | HCID 191408 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | (1-Benzyl-4-phenylpiperidine-4-carbonyl)-oxidoazanium | HCID 88146759 | — |
反応手順
Combine 1-benzyl-4-phenyl-4-cyanopiperidine (535 g, 1940 mmol), aqueous sodium hydroxide (85 mL, 50% by weight), and ethanol (5 L). Heat to 50° C. Remove the heating and add a solution of hydrogen peroxide (856 mL, 30% by weight in water) at such a rate that the temperature of the reaction mixture does not rise above 50° C. After the addition of hydrogen peroxide is complete, maintain the temperature of reaction mixture at 50° C. After 20 hours, dilute the reaction mixture with water (3 L) and concentrate invacuo at 35° C. to remove the ethanol. Cool the reaction mixture to ambient temperature to give a solid. Collect the solid by filtration, rinse with water, and air dried to give 1-benzyl-4-phenylpiperidine-4-carboxylic acid amide N-oxide.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05861417 |
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| 出典データセット | uspto-grants-1999_01 |
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| ORD ID | ord-0da2ce208f80494cb708abb7faf67f4b |
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| 出典メモ | uspto-grants-1999_01 |
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