反应详情

温度

100 °C

To the thus obtained 2-(4-methyl-1-piperazinyl)-3,6-difluoro-4-chloro-5-nitrotoluene (0.13 g) are added anhydrous dimethylformamide (2 ml), potassium fluoride (37 mg) and cyclopropylamine (0.15 ml) and the mixture is stirred at 100° C. for 3 hours. After cooling, the reaction mixture is poured into ice-water, extracted with dichloromethane and the extract is dried. The solvent is distilled off under reduced pressure and purified by silica-gel column-chromatography (eluent; dichloromethane : methanol=10 : 1) to give 3-(4-methyl-1-piperazinyl)-4-fluoro-5-chloro-2-methyl-6 -nitro-N-cyclopropylaniline (0.14 g).

1. temperatureAfter cooling
2. extractionextracted with dichloromethane
3. customthe extract is dried
4. distillationThe solvent is distilled off under reduced pressure
5. custompurified by silica-gel column-chromatography (eluent; dichloromethane : methanol=10 : 1)