反应 #586156

反应方程式

water

3-trifluoromethylpyrazole

2-chloro-4-fluorobenzonitrile

potassium carbonate

→

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

收率 92.0%

溶剂

N,N-dimethylformamide

反应条件

后处理

1. 1
   萃取the organic matters were extracted with 50 ml of ethyl acetate twice
2. 2
   洗涤washed with 50 ml of water twice
3. 3
   干燥dried over anhydrous magnesium sulfate
4. 4
   workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure
5. 5
   洗涤After washed with n-hexane

实验过程

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.

来源