HCID 18995948, compound → 4-Amino-2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole

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Reaction Steps

84 g of 4-nitro-2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole from Example 7 were dissolved in 500 ml of tetrahydrofuran and hydrogenated with 15-20 bar of hydrogen for 5 hours at room temperature on 5 g of palladium-on-charcoal (5%). The mixture was then filtered and the filtrate was concentrated and distilled under vacuum. The yield was 31 g (40% of theory) and the boiling point was 70° C. at 0.1 mbar. The NMR spectra showed the following characteristic absorptions: 19F NMR: -68.6 and -81.5 ppm. 1H NMR: 4.69 ppm.

Provenance & Evidence