Reacción #53589

Ecuación de reacción

water

3-trifluoromethylpyrazole

2-chloro-4-fluorobenzonitrile

potassium carbonate

→

2-chloro-4-(3-trifluoromethylpyrazolyl)benzonitrile

Rendimiento 92.0%

Disolventes

N,N-dimethylformamide

Condiciones de reacción

Tratamiento posterior

1. 1
   Extracciónthe organic matters were extracted with 50 ml of ethyl acetate twice
2. 2
   Lavadowashed with 50 ml of water twice
3. 3
   Secadodried over anhydrous magnesium sulfate
4. 4
   workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure
5. 5
   LavadoAfter washed with n-hexane

Procedimiento

2.5 g (18.4 mmol) of 3-trifluoromethylpyrazole, 2.9 g (18.4 mmol) of 2-chloro-4-fluorobenzonitrile and 2.8 g (20.2 mmol) of potassium carbonate in 20 ml of N,N-dimethylformamide were stirred at 60° C. for 2 hours. After cooling to room temperature, the reaction mixture was poured into 100 ml of water, and the organic matters were extracted with 50 ml of ethyl acetate twice. The ethyl acetate layers were combined, washed with 50 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. After washed with n-hexane, the residue afforded 4.6 g of 2-chloro-4-(3-trifluoromethylpyrazolyl)benzonitrile (yield 92.0%) as a white powder, which was used in Reference Example 3 as the starting material.

Fuente