関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hexamethylphosphoramide | HCID 12679 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | HCID 23693872 | HCID 23693872 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Desethyl-etomidate | HCID 297427 | — |
反応手順
A mixture of 14.3 parts of (-)-1-(1-phenylethyl)-1H-imidazole-5-carboxylic acid sodium salt, 1.9 parts of a 61.8% suspension of sodium hydride in mineral oil and 60 parts of hexamethylphosphoric triamide is stirred for 20 hours at 100° C. under Argon atmosphere. The mixture is allowed to cool to room temperature and poured onto 150 parts of water. The whole is washed three times with 200 parts of dichloromethane. The aqueous phase is neutralized (pH 7) with acetic acid and the product is allowed to crystallize. The product is filtered off, dried and recrystallized from ethanol, yielding (±)-1-(1-phenylethyl)-1H-imidazole-5-carboxylic acid; m.p. 188° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04038286 |
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| 出典データセット | uspto-grants-1977_07 |
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| ORD ID | ord-a66ebd993bca4849b5efc0f60599907f |
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| 出典メモ | uspto-grants-1977_07 |
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