反应详情

To a solution (50 mL) of 2-[2-bromo-4-(cyclopropylmethoxy)phenyl]-N-methoxy-N-methylacetamide (3.00 g) in THF was added dropwise methylmagnesium bromide (19.6 mL, 1.4 M, a mixed solution of toluene-diethyl ether (3/1)) under ice-cooling. The mixture was stirred at room temperature for 3 hr, poured into saturated aqueous ammonium chloride solution, and extracted with ethyl acetate. The obtained organic layer was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to give the title compound as a colorless oil (1.29 g).

1. extractionextracted with ethyl acetate
2. washThe obtained organic layer was washed with saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. customthe solvent was evaporated under reduced pressure
5. customThe residue was purified by silica gel column chromatography (hexane/ethyl acetate)