反应详情

To 2,3,6-trifluoro-4-chloro-5-nitrotoluene (0.17 g) are added ethanol (3.3 ml), water (0.5 ml), N-methylpiperazine (0.45 ml) and triethylamine (0.56 ml) and the mixture is refluxed for 24 hours. After the reaction is completed, water is added to the reaction mixture and the mixture is extracted with diethyl ether, and the extract is washed with water and dried. The solvent is distilled off under reduced pressure and the residue is purified by silica-gel column-chromatography (eluent; dichloromethane: methanol=20 : 1) to give 2-(4-methyl-1-piperazinyl)-3,6-difluoro-4-chloro-5-nitrotoluene (0.13 g).

1. temperaturethe mixture is refluxed for 24 hours
2. extractionthe mixture is extracted with diethyl ether
3. washthe extract is washed with water
4. customdried
5. distillationThe solvent is distilled off under reduced pressure
6. customthe residue is purified by silica-gel column-chromatography (eluent; dichloromethane: methanol=20 : 1)