化工社化工社 化学情報印刷レポート · 研究参考用
Diisopropylethylamine → 1-(2-fluoro-4-nitrophenyl)-4-methyl-1H-imidazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1,2-Difluoro-4-nitrobenzene | HCID 123053 | — |
| 反応物 | HCID 178418800 | HCID 178418800 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-(2-fluoro-4-nitrophenyl)-4-methyl-1H-imidazole | HCID 21876596 | — |
反応手順
4-Methylimidazole (45.1 g, 0.55 M) and N,N-diisopropylethylamine (161 g, 1.25 M) were dissolved in acetonitrile (800 ml), and 3,4-difluoronitrobenzene (79.5 g, 0.5 M) added. The mixture was stirred and heated to reflux under nitrogen for 24 hours. Solvent was evaporated, the residue dissolved in ethyl acetate (800 ml), washed with water (400 ml), brine (200 ml), and dried (magnesium sulfate). The residue was dissolved in toluene (250 ml), treated with charcoal, filtered, and diluted with hot cyclohexane (75 ml) to crystallise 3-fluoro-4-(4-methylimidazol-1-yl)nitrobenzene (64.7 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07087629B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-dc7b9a5830914572958c7fec79e92c2d |
| 出典メモ | uspto-grants-2006_08 |