反应详情

温度

35 °C

At 25° C., 6.83 g (0.02 mole) 4-chloro-3-(2,5-difluoro-4-nitrophenyl)-1-methyl-5-(trifluoromethyl)-1H-pyrazole, 4.1 g (0.03 mole) K2CO3, 3.1 mL (0.03 mole) N-methyl-N-propylamine and a catalytic amount of CuF2 were slurried in 50 mL 1-methyl-2-pyrrolidinone. The reaction mixture was stirred at 35° C. for 2 hours. The mixture was cooled, diluted with 100 mL cold water, and extracted four times with ethyl acetate. The ethyl acetate extracts were washed with brine, dried over anhydrous MgSO4, and stripped in vacuo. The residue was purified chromatographically using 15% ethyl acetate in hexane as the eluent to give 6.8 g (86%) of 5-(4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl)-4-fluoro-N-methyl-2-nitro-N-propylbenzeneamine as an orange oil, nD25 1.5534.

1. customAt 25° C.
2. temperatureThe mixture was cooled
3. extractionextracted four times with ethyl acetate
4. washThe ethyl acetate extracts were washed with brine
5. dry with materialdried over anhydrous MgSO4
6. customThe residue was purified chromatographically