関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 2-Bromo-1-(3,4-dimethoxyphenyl)ethan-1-one | HCID 270423 | — |
| 反応物 | Cyclopropanecarboximidamide | HCID 431751 | — |
| 生成物 | HCID 178418803 | HCID 178418803 | — |
反応手順
Ex-105A: A solution of 2-bromo-1-(3,4-dimethoxy-phenyl)-ethanone (0.3 g, 1.16 mmol), cyclopropanecarboxamidine (0.14 g, 1.16 mmol) and sodium hydroxide (0.18 g, 4.5 mmol) in ethanol was refluxed overnight. The solvent was removed under reduced pressure, the residue taken up to water. The aqueous solution was then extracted with dichloromethane which was subsequently washed with brine, dried over sodium bicarbonate and concentrated. The crude product was purified by flash chromatography. Elution with ethyl acetate (50%, v/v, in hexane) then methanol (10%, v/v in dichloromethane) afforded 2-cyclopropyl-4-(2,4-dimethoxy-phenyl)-1H-imidazole as white solid (0.1 5 g, 53%): 1HNMR (CDCl3) δ 9.50 (bs, 1H), 7.63 (s, 1H), 7.20 (s, 1H), 6.57–6.53 (m, 2H), 3.93 (s, 3H), 3.03 (s, 3H), 1.97–1.93 (m, 1H), 1.00–0.94 (m, 4H). MS m/z=245 ([M+H]+, 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US07094801B2 |
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| 出典データセット | uspto-grants-2006_08 |
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| ORD ID | ord-bbb2cd7fd873464ea1dfd997d79efdb3 |
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| 出典メモ | uspto-grants-2006_08 |
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