反应详情

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 over 5 g of palladium-oncharcoal (5% strength) at room temperature for 5 hours. The mixture was then filtered, the filtrate was concentrated and the residue was distilled in vacuo. The yield was 31 g (40% of theory), and the boiling point was 70° C. under 0.1 mbar. The NMR spectra showed the following characteristic absorptions: 19F-NMR: -68.6 and -81.5 ppm. 1H-NMR: 4.69 ppm.

1. filtrationThe mixture was then filtered
2. concentrationthe filtrate was concentrated
3. distillationthe residue was distilled in vacuo