関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methoxybenzenecarboximidamide | HCID 229074 | — |
| 反応物 | 2-Bromo-2'-nitroacetophenone | HCID 244025 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 2-(4-Methoxyphenyl)-4-(2-nitrophenyl)imidazole | HCID 178488923 | 78.1% |
反応手順
A mixture of 2-bromo-2'-nitroacetophenone (18 g), 4-methoxybenzamidine (20 g), and silica gel (20 g) in acetonitrile (500 ml) is heated at 40° C. for 24 hours. The reaction is evaporated and the residue put on a layer of silica gel and eluted with 50% ethyl acetate/hexane (1500 ml). The solution is evaporated under reduced pressure to approximately 250 ml and extracted with 5% HCl (3×250 ml) . The combined aqueous solution is basified with K2CO3 and extracted with ethyl acetate (3×400 ml) to afford 2-(4-methoxyphenyl)-4-(2-nitrophenyl)-imidazole (17 g) as a dark yellow oil which is used in the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US06103731 |
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| 出典データセット | uspto-grants-2000_08 |
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| ORD ID | ord-0268b124d7274ac985604a8b37b9ab91 |
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| 出典メモ | uspto-grants-2000_08 |
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