反应详情

64 g of 4-methyl-2-(1-chloro-2,2,2-trifluoroethyl)-2-trifluoromethyl-1,3-benzodioxole from Example 9 were dissolved in 500 ml of carbon tetrachloride, and 36 g of N-bromosuccinimide and 0.5 g of AIBN (azoisobutyronitrile) were added. The mixture was stirred under reflux for 3 hours and then cooled and filtered. The solvent was stripped off and the residue was distilled in vacuo. The yield was 57 g (71% of theory), and the boiling point was 80°-82° C. under 0.1 mbar. The NMR spectra showed the following characteristic absorptions: 1H-NMR: 4.72 ppm.

1. temperatureunder reflux for 3 hours
2. temperaturecooled
3. filtrationfiltered
4. distillationthe residue was distilled in vacuo