反应详情

温度

120 °C

7.68 g of sodium hydride dispersion (ca. 50 percent in mineral oil) was washed with pentane under nitrogen and 100 ml of N,N-dimethylformamide was then added. 21.92 g (135 mmol) of 3-(trifluoromethyl)phenol was added dropwise over 30 minutes at room temperature. The resultant phenate solution was added dropwise over 2 hours, under nitrogen, to a solution of 20.1 g (136 mmol) of 2,3-dichloropyridine in 80 ml of N,N-dimethylformamide, heated to 120° C. After a reaction time of 3 hours, the mixture was cooled to room temperature, the precipitate of sodium chloride was filtered off and the filtrate was concentrated. The residue was extracted with toluene and 0.1 N hydrochloric acid and the organic phase was washed with saturated sodium chloride solution and concentrated. The oily residue was distilled under vacuum. The yield of the title compound was 24.75 g (67 percent) of a colorless oil, content (GC) 99.7 percent. Other data concerning the title compound was:

1. wash7.68 g of sodium hydride dispersion (ca. 50 percent in mineral oil) was washed with pentane under nitrogen
2. addition100 ml of N,N-dimethylformamide was then added
3. temperatureAfter a reaction time of 3 hours, the mixture was cooled to room temperature
4. filtrationthe precipitate of sodium chloride was filtered off
5. concentrationthe filtrate was concentrated
6. extractionThe residue was extracted with toluene and 0.1 N hydrochloric acid
7. washthe organic phase was washed with saturated sodium chloride solution
8. concentrationconcentrated
9. distillationThe oily residue was distilled under vacuum