反应详情

温度

60 °C

A mixture of 250 ml of 100% strength by weight nitric acid and 350 ml of concentrated sulphuric acid was added to an initial charge of 352 g of 5-nitro-2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole from Example 16a. The mixture was stirred for 2 hours at 60° C. It was cooled, poured into ice-water and extracted with methylene chloride. After washing the mixture with sodium hydrogen carbonate solution and drying it was concentrated on a rotary evaporator. The yield was 392 g (91% of theory), the melting point was 125° C. The NMR spectra showed the following characteristic absorptions: 19F-NMR: -68.5 and -81.0 ppm; 1H-NMR: 4.86 ppm.

1. additionwas added to
2. temperatureIt was cooled
3. extractionextracted with methylene chloride
4. washAfter washing the mixture with sodium hydrogen carbonate solution
5. customdrying it
6. concentrationwas concentrated on a rotary evaporator