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

Participants

Reaction Steps

A solution of 54.4 g of 2-(2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole in 75 ml of methylene chloride was added dropwise to a mixture of 40 ml of 65% strength by weight nitric acid and 40 ml of concentrated sulphuric acid at i0° C. The mixture was subsequently stirred at room temperature for 1 hour and then poured onto ice-water, the organic phase was separated off and the aqueous phase was extracted with methylene chloride. The combined organic phases were washed with water, dried and freed from readily volatile constituents. 95 g of the product (=86% of theory) with a melting point of 87° to 88° C. remained.

Provenance & Evidence