反应详情

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).

1. temperatureheated
2. temperatureto reflux under nitrogen for 24 hours
3. customSolvent was evaporated
4. dissolutionthe residue dissolved in ethyl acetate (800 ml)
5. washwashed with water (400 ml), brine (200 ml)
6. dry with materialdried (magnesium sulfate)
7. dissolutionThe residue was dissolved in toluene (250 ml)
8. additiontreated with charcoal
9. filtrationfiltered
10. additiondiluted with hot cyclohexane (75 ml)
11. customto crystallise 3-fluoro-4-(4-methylimidazol-1-yl)nitrobenzene (64.7 g)