反应详情

N,N-Diisopropylethylamine (11.5 ml) and 1-methyl-2-oxopiperazine (4.12 g) were added to a solution of 3,4-difluoronitrobenzene (1.82 ml) in acetonitrile (100 ml), and the mixture heated to reflux for 16 hours. Solvent was evaporated, and the residue chromatographed on silica, using as eluant a gradient increasing in polarity from 0 to 100% ethyl acetate in iso-hexane. Relevant fractions were combined and evaporated to give 3-fluoro-4-(4-methyl-3-oxopiperazin-1-yl)nitrobenzene (3.37 g).

1. temperaturethe mixture heated
2. temperatureto reflux for 16 hours
3. customSolvent was evaporated
4. customthe residue chromatographed on silica
5. temperaturea gradient increasing in polarity from 0 to 100% ethyl acetate in iso-hexane
6. customevaporated