反应详情

温度

85 °C

15.1 g (0.0752 mol, 96.5% pure) of 3-difluoromethyl-1-methyl-1H-pyrazole-4-carbonyl chloride were dissolved at 25° C. in 100 ml of toluene. The solution was evacuated to 350 mbar and heated to 85° C. Subsequently, within 60 min, 20 g (0.074 mol, 75%; 65:10 syn/anti isomer mixture) of 9-isopropyl-1,2,3,4-tetrahydro-1,4-methanonaphthalen-5-ylamine, dissolved in 100 ml of toluene, were metered in and the reaction mixture was stirred for another 1 hour. After venting and cooling to 25° C., the mixture was stirred overnight. Subsequently, the mixture was concentrated under reduced pressure and dried. The yield was 31.3 g; according to 1H NMR 70% pure (82%).

1. customThe solution was evacuated to 350 mbar
2. temperaturecooling to 25° C.
3. stirringthe mixture was stirred overnight
4. concentrationSubsequently, the mixture was concentrated under reduced pressure
5. customdried