Nitric Acid → 2-(1-Chloro-2,2,2-trifluoroethyl)-5,6-dinitro-2-(trifluoromethyl)-1,3-benzodioxole

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Reaction Conditions

Reaction Steps

352 g of 5-nitro-2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole from Example 28 were initially introduced into the reaction vessel and a mixture of 250 ml of 100% strength by weight nitric acid and 350 ml of concentrated sulphuric acid was added. The mixture was stirred at 60° C. for 2 hours. After cooling, it was poured onto ice-water and extracted with methylene chloride. After washing with sodium bicarbonate solution and drying, the extract was evaporated on a rotary evaporator. The yield was 392 g (91% of theory), and 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.

Provenance & Evidence