関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 1-(3-Fluoro-4-methoxyphenyl)ethan-1-one | HCID 96828 | — |
| 反応物 | o-(3-Fluorobenzyl)hydroxylamine hydrochloride | HCID 23206139 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 3'-Fluoro-4'-methoxyacetophenone-o-3-fluorobenzyloxime | HCID 87138665 | 90.1% |
反応手順
A solution of 3-fluoro-4-methoxyacetophenone (0.063 g, 0.377 mmol), O-(3-fluorobenzyl)hydroxylamine hydrochloride (0.100 g, 0.569 mmol) and pyridine (0.14 ml, 1.73 mmol) in ethanol (5 ml) was stirred at reflux under nitrogen for 4 h and cooled to room temperature. The solution was concentrated to a pale yellow oil which was diluted with water. The suspension was extracted with dichloromethane (×3). The combined organic phases were washed with water and brine, dried over magnesium sulphate, filtered and concentrated to a white solid. The crude product was purified by column chromatography (SiO2), eluting with 95:5 petrol/ethyl acetate, to give 3′-fluoro-4′-methoxyacetophenone-O-3-fluorobenzyloxime (CP9-126) as a white solid (0.099 g, 90%), m.p. 67°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08536157B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-5b90820628314994913bf3c02418e6c9 |
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| 出典メモ | uspto-grants-2013_09 |
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