反应详情

温度

85 °C

100.0 g (0.504 mol, 98% pure) of 3-difluoromethyl-1-methyl-1H-pyrazole-4-carbonyl chloride were dissolved at 25° C. in 257.2 g of toluene. The solution was evacuated to 400 mbar and heated to 85° C. Subsequently, within 3 hours, 492.8 g (0.499 mol, 23% strength) of toluenic 3′,4′,5′-trifluorobiphenyl-2-ylamine solution were metered in, after which stirring was continued for another 1 hour. After venting and cooling to 25° C. with a ramp of 10° C./h, the mixture was stirred overnight. Subsequently, the mixture was cooled to 0° C., and the solid constituents were filtered off, washed with cold toluene and dried at 80° C. under reduced pressure. The yield (without further processing of the mother liquor) was 177.7 g (92%).

1. customThe solution was evacuated to 400 mbar
2. waitwas continued for another 1 hour
3. temperaturecooling to 25° C. with a ramp of 10° C./h
4. stirringthe mixture was stirred overnight
5. temperatureSubsequently, the mixture was cooled to 0° C.
6. filtrationthe solid constituents were filtered off
7. washwashed with cold toluene
8. customdried at 80° C. under reduced pressure
9. customThe yield (without further processing of the mother liquor)