関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Idramantone | HCID 64184 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 5-Hydroxy-adamantan-2-one oxime | HCID 23008983 | 71% |
反応手順
5-Hydroxyadmantan-2-one (TCI America, Portland, Oreg.; 3 g, 18.0 mmol) was dissolved in EtOH (20 mL) and the solution was added to a solution of hydroxylamine hydrochloride (12 g, 172.7 mmol) in 1N NaOH (16 mL). The mixture was heated at 100° C. for 1 hour. The EtOH was evaporated, and water and DCM were added. The separated aqueous layer was further extracted twice with DCM. The combined DCM layers were evaporated under vacuum. Crystallization from EtOAc gave 5-hydroxy-adamantan-2-one oxime (2.3 g, 71%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07645773B2 |
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| 出典データセット | uspto-grants-2010_01 |
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| ORD ID | ord-fd671fa92bdc40ee886bca327b613883 |
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| 出典メモ | uspto-grants-2010_01 |
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