Nitric Acid → 5-Nitro-2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxol

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Reaction Steps

613 g of 2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole of Example 2a were dissolved in 1.2 l of methylene chloride and the solution was added dropwise at 0° to 10° C. to a mixture of 400 ml of 65% strength nitric acid and 400 ml of concentrated sulphuric acid. Stirring was continued for 2 hours at room temperature. Then, the mixture was poured carefully into 2 l of ice-water and extracted using methylene chloride. The combined organic phases were washed twice using water, dried and concentrated. The yield was 652 g (93% of theory). The NMR spectra showed the following characteristic absorptions: 19F-NMR: -66.4 and -79.2 ppm. 1H-NMR: 4.81 ppm.

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