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Hydroxyamine hydrochloride → 1-(2',4'-Dichloro-biphenyl-4-yl)-6-hydroxy-hexan-1-one oxime
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydroxyamine hydrochloride | HCID 443297 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 反応物 | 1-(2',4'-Dichloro-biphenyl-4-yl)-6-hydroxy-hexan-1-one | HCID 24896595 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(2',4'-Dichloro-biphenyl-4-yl)-6-hydroxy-hexan-1-one oxime | HCID 74424212 | — |
反応手順
1-(2′,4′-Dichloro-biphenyl-4-yl)-6-hydroxy-hexan-1-one (400 mg) was dissolved in a mixture of ethanol (10 mL) and water (5 mL). Hydroxylamine hydrochloride (300 mg) and sodium acetate (350 mg) were added and the mixture refluxed for 5 hours. After cooling, the mixture was diluted with water and extracted with ethyl acetate. Evaporation and recrystallisation from ether/petrol gave the title compound as a white solid. 13C NMR (CDCl3): δ 25.9, 26.2, 26.2, 32.3, 62.8, 126.1, 127.3, 129.6, 129.8, 132.0, 133.2, 134.0, 135.2, 138.4, 139.1 and 159.3. 1H NMR (CDCl3): δ 1.45 (2H, m), 1.59 (4H, m), 2.80 (2H, m), 3.62 (2H, m), 7.26 (2H, m), 7.41 (2H, d, J=7.0 Hz), 7.47 (1H, m) and 7.64 (2H, d, J=7.0 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07560597B2 |
| 出典データセット | uspto-grants-2009_07 |
| ORD ID | ord-79dacc81815348a391fc0b688926d642 |
| 出典メモ | uspto-grants-2009_07 |