5-Nitro-2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxol → HCID 54242850, compound

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Reaction Steps

72 g of 5-nitro-2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole from Example 28 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 solvent was stripped off under vacuum. The yield was 60 g (93% of theory) and the boiling point was 80°-82° C. at 0.1 mbar. The NMR spectra showed the following characteristic absorptions: 19F NMR: -66.5 and -79.4 ppm. 1H NMR: 4.68 ppm.

Provenance & Evidence