反应详情

温度

85 °C

79.1 g (0.494 mol, 99% pure) of 1,3-dimethyl-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, 483.0 g (0.489 mol, 23% strength) of toluenic 3′,4′,5′-trifluorobiphenyl-2-ylamine solution were metered in and the reaction mixture was stirred for a further 1 hour. After venting and cooling to 70° C., the mixture was cooled to 20° C. with a cooling ramp of 5° C./h and stirred overnight. Subsequently, the mixture was cooled to 0° C., and the solids 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 155.4 g (92%).

1. customThe solution was evacuated to 400 mbar
2. temperaturecooling to 70° C.
3. temperaturethe mixture was cooled to 20° C. with a cooling ramp of 5° C./h
4. stirringstirred overnight
5. temperatureSubsequently, the mixture was cooled to 0° C.
6. filtrationthe solids 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)