反应详情

温度

-78 °C

To a tetrahydrofuran (100 ml) solution of 1,3-difluoro-5-methoxybenzene (7 g, 48.6 mmol) was added 1.6 M hexane solution of n-butyllithium (30 ml, 48.6 mmol) dropwise at −78° C. over 30 minutes and the mixture was stirred for 2 hours at −78° C. 1,1,1-Trifluoroacetone (6.5 g, 58.3 mmol) was added at −78° C. and the mixture was stirred for 2 hours at −78° C. followed by additional stirring for 1 hour at room temperature. Then, the reaction was diluted with water and the product was extracted with ethyl acetate. Then, the organic layer was filtrated, evaporated and concentrated. The residue was purified by silica gel column chromatography, eluting with hexane/ethyl acetate (10:1), to furnish 9.7 g (78% yield) of the title compound as a colorless oil.

1. stirringthe mixture was stirred for 2 hours at −78° C.
2. stirringby additional stirring for 1 hour at room temperature
3. extractionthe product was extracted with ethyl acetate
4. filtrationThen, the organic layer was filtrated
5. customevaporated
6. concentrationconcentrated
7. customThe residue was purified by silica gel column chromatography
8. washeluting with hexane/ethyl acetate (10:1)