反应详情

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 at 10° C. to a mixture of 40 ml of 65% strength by weight nitric acid and 40 ml of concentrated sulphuric acid. Stirring was continued for 1 hour at room temperature and the batch was then poured into ice-water, the organic phase was separated off, and the aqueous phase was extracted using methylene chloride. The combined organic phases were washed with water, dried and freed from volatile components. 95 g of the product (=86% of theory), which had a melting point of 87° to 88° C., remained. The NMR spectra showed the following characteristic absorptions: 19F-NMR: -59.0 and -69.4 ppm. 1H-NMR: 3.10 ppm.

1. customthe organic phase was separated off
2. extractionthe aqueous phase was extracted
3. washThe combined organic phases were washed with water
4. customdried