반응 #8251

반응 방정식

4-Methylimidazole

N,N-diisopropylethylamine

3,4-difluoronitrobenzene

→

3-Fluoro-4-(4-methylimidazol-1-yl)nitrobenzene

용매

acetonitrile

반응 조건

후처리

1. 1
   온도heated
2. 2
   온도to reflux under nitrogen for 24 hours
3. 3
   기타Solvent was evaporated
4. 4
   workup.DISSOLUTIONthe residue dissolved in ethyl acetate (800 ml)
5. 5
   세척washed with water (400 ml), brine (200 ml)
6. 6
   건조dried (magnesium sulfate)
7. 7
   workup.DISSOLUTIONThe residue was dissolved in toluene (250 ml)
8. 8
   workup.ADDITIONtreated with charcoal
9. 9
   여과filtered
10. 10
    workup.ADDITIONdiluted with hot cyclohexane (75 ml)
11. 11
    기타to crystallise 3-fluoro-4-(4-methylimidazol-1-yl)nitrobenzene (64.7 g)

실험 절차

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).

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