反应详情

24.0 g (0.09 mol) of 2,2,2-trifluoro-1-(4-trifluoromethoxyphenyl)ethanol and 1.57 g (0.0046 mol) of tetrabutylammonium hydrogen sulfate are dissolved in 250 ml of methylene chloride at room temperature. 100 ml (0.12 mol) of an approximately 12% strength sodium hypochlorite solution are metered in within 20 minutes with vigorous stirring and the mixture is stirred for a further 5 hours during which the temperature rises to 40° C. The reaction mixture is added to 400 ml of water, the phases are separated, the aqueous phase is extracted several times with methylene chloride and the combined organic phases are washed with saturated aqueous sodium chloride solution. After drying the organic phase with sodium sulfate, the volatiles are distilled off. Following distillation of the crude product in a kugelrohr (14 torr, bath temperature 100°-115° C.), 17.19 g (74% of theory) of 4-trifluoroacetyltrifluoromethoxybenzene are obtained. nD20 : 1.4188.

1. customare metered in within 20 minutes
2. stirringthe mixture is stirred for a further 5 hours during which the temperature
3. customrises to 40° C
4. customthe phases are separated
5. extractionthe aqueous phase is extracted several times with methylene chloride
6. washthe combined organic phases are washed with saturated aqueous sodium chloride solution
7. dry with materialAfter drying the organic phase with sodium sulfate
8. distillationthe volatiles are distilled off
9. distillationdistillation of the crude product in a kugelrohr (14 torr, bath temperature 100°-115° C.), 17.19 g (74% of theory) of 4-trifluoroacetyltrifluoromethoxybenzene
10. customare obtained