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 from Example 2 were dissolved in 1.2 1 of methylene chloride and the solution was added dropwise to a mixture of 400 ml of 65% strength nitric acid and 400 ml of concentrated sulphuric acid at 0°-10° C. The mixture was subsequently led at room temperature for 2 hours. It was then poured carefully onto 2 1 of ice-water and extracted with methylene chloride. The combined organic phases were washed twice with 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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