関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Hydroxide | HCID 14923 | — |
| 反応物 | Phosphorus oxychloride | HCID 24813 | — |
| 反応物 | 5-(3-benzenesulfonylpropyl)-1-butyl-1H-pyrazole-3-carboxamide | HCID 66959024 | — |
| 生成物 | 5-(3-benzenesulfonylpropyl)-1-butyl-1H-pyrazole-3-carbonitrile | HCID 66958321 | 86.5% |
反応手順
Phosphorus oxychloride (25 mL) was added to 5-(3-benzenesulfonylpropyl)-1-butyl-1H-pyrazole-3-carboxamide (10.4 g, 30.0 mmol) and heated to 90° C. for 2.5 hours. The reaction mixture was then cooled to ambient temperature and poured into ice water cooled by an ice bath. Additional ice was added to the reaction mixture and the pH of the mixture was adjusted to 8-9 by addition of 30% saturated aqueous ammonium hydroxide. The mixture was extracted with ethyl acetate and the combined organic layers were dried over magnesium sulfate, filtered, and concentrated under reduced pressure to afford 8.60 g of 5-(3-benzenesulfonylpropyl)-1-butyl-1H-pyrazole-3-carbonitrile.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07879849B2 |
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| 出典データセット | uspto-grants-2011_02 |
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| ORD ID | ord-c0cbdfafe9b446d6813b86115aa52c86 |
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| 出典メモ | uspto-grants-2011_02 |
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