反应详情

温度

140 °C

A mixture of 2-nitrophenol (18.8 g, 135 mmol), 2,2,2-trifluoroethyl para-toluenesulfonate (34.36 g, 135 mmol), potassium carbonate (18.7 g, 135 mmol) and DMF (200 mL) was heated 16 hours at 140° C. The reaction mixture then was cooled, diluted with water (600 mL) and extracted with ether/hexanes (1:1; 3×400 mL). The combined extracts were washed with saturated sodium bicarbonate (3×100 mL) and brine, dried (Na2SO4), filtered and concentrated to give 1-(2,2,2-trifluoroethoxy)-2-nitrobenzene (27 g, 117 mmol) as an oil.

1. temperatureThe reaction mixture then was cooled
2. extractionextracted with ether/hexanes (1:1; 3×400 mL)
3. washThe combined extracts were washed with saturated sodium bicarbonate (3×100 mL) and brine
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated