化工社化工社 化学情報印刷レポート · 研究参考用
2-Methylimidazole → 1-(2-fluoro-4-nitrophenyl)-2-methyl-1H-imidazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Methylimidazole | HCID 12749 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 1,2-Difluoro-4-nitrobenzene | HCID 123053 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-(2-fluoro-4-nitrophenyl)-2-methyl-1H-imidazole | HCID 21876645 | 52% |
反応手順
2-Methylimidazole (9.02 g, 0.11 M) and N,N-diisopropylethylamine (32.2 g, 0.25 M) were dissolved in acetonitrile (160 ml), and 3,4-difluoronitrobenzene (15.9 g, 0.1 M) added. The mixture was stirred and heated to reflux under nitrogen for 24 hours. Solvent was evaporated, the residue dissolved in ethyl acetate (300 ml), washed with water (150 ml), brine (150 ml), and dried (magnesium sulfate). The residue was recrystallised from a mixture of ethyl acetate (25 ml) and cyclohexane (150 ml) with the addition of charcoal to give the title compound (11.5 g), mp 106–107°.
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-29e51974d6614de39e82ca9826379728 |
| 出典メモ | uspto-grants-2006_08 |