反应详情

To 3-ethyl-2,4,5-trifluoro-nitrobenzene (1.02 g) are added ethanol (4.5 ml) and water (0.5 ml) and the mixture is stirred. To the mixture is added with stirring a mixture of 1-methylpiperazine (0.83 ml), triethylamine (1.0 ml) and ethanol (0.6 ml), and the mixture is refluxed for 5 hours. To the reaction mixture is further added 1-methylpiperazine (1.0 ml), and the mixture is refluxed for 3 hours. The mixture is concentrated under reduced pressure, and the resulting residue is purified by silica gel column chromatography (solvent, methylene chloride) to give 3-ethyl-2,5-difluoro-4-(4-methyl-1-piperazinyl)nitrobenzene (1.12 g), as yellow oil.

1. additionTo the mixture is added
2. stirringwith stirring
3. temperaturethe mixture is refluxed for 5 hours
4. temperaturethe mixture is refluxed for 3 hours
5. concentrationThe mixture is concentrated under reduced pressure
6. customthe resulting residue is purified by silica gel column chromatography (solvent, methylene chloride)