関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Tetralone | HCID 10724 | — |
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N-(3,4-dihydro-2H-naphthalen-1-ylidene)hydroxylamine | HCID 76876 | 63.9% |
反応手順
To a solution of α-tetralone (100.0 g, 0.68 mol) in 300 mL of methanol was added hydroxylamine hydrochloride (71.0 g, 1.03 mol) and the resulting solution was stirred at reflux for 2 hours. The mixture was allowed to cool to 20-24° C. and was concentrated under reduced pressure. The resulting mixture was diluted with 1 L of water and extracted with dichloromethane. The organic layer was washed with saturated aqueous sodium chloride, dried over sodium sulfate, filtered and concentrated under reduced pressure. The residue was crystallized from isopropanol to provide 70.0 g (63%) of the desired compound as an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06743785B2 |
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| 出典データセット | uspto-grants-2004_06 |
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| ORD ID | ord-54e1e56f3d4d41a199e6f95cff67b043 |
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| 出典メモ | uspto-grants-2004_06 |
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