反应详情

温度

90 °C

To 10 □ of 1,2-dichloroethane were added 1.0 g of 2,4,5-trifluorobenzonitrile, 0.43 g of zinc chloride, and 1.3 g of potassium ethylmalonate, and then the mixture was stirred at reflux. After the reaction was completed, 11 □ of 6 N hydrochloric acid was added to the mixture, which then was stirred at reflux at 90° C. for 1 hour. After confirming completion of the reaction by TLC, the solution was cooled to 20° C., and then an organic layer was separated therefrom. The organic layer was concentrated through distillation under reduced pressure. Thus resulted residue was purified by silica gel column chromatography (eluent: ethylacetate/n-hexane=1/10, v/v) to obtain the title compound in the yield of 80% (1.2 g).

1. temperatureat reflux
2. stirringthen was stirred
3. customcompletion of the reaction by TLC
4. temperaturethe solution was cooled to 20° C.
5. customan organic layer was separated
6. concentrationThe organic layer was concentrated through distillation under reduced pressure
7. customThus resulted residue was purified by silica gel column chromatography (eluent