反应详情

To a solution of 2-chloro-1-(methoxymethoxy)-3-(trifluoromethyl)benzene (11.8 g) in THF (100 mL) was added dropwise n-butyllithium (2.5M hexane solution) (21.0 mL) at −10° C., and the mixture was stirred for 2 hr. Then, to the reaction mixture was added dropwise a solution of methyl chloroformate (23.0 g) in THF (50.0 mL), and the mixture was stirred at 10° C. for 16 hr. The reaction mixture was poured into saturated aqueous sodium bicarbonate solution, and the mixture was extracted with ethyl acetate (×2). The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by flash silica gel column chromatography (ethyl acetate/petroleum ether) to give the title compound (6.00 g).

1. stirringthe mixture was stirred at 10° C. for 16 hr
2. extractionthe mixture was extracted with ethyl acetate (×2)
3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
4. customthe solvent was evaporated under reduced pressure
5. customThe residue was purified by flash silica gel column chromatography (ethyl acetate/petroleum ether)