反应详情

Et3SiH (8.5 mL, 0.0531 mol) was added to a mixed solution of chloroform (8 mL) and acetonitrile (32 mL) of (4-methoxy-2-methyl phenyl)(4-methylphenyl)methanone and BF3.Et2O (4.5 mL, 0.0354 mol) was added dropwise while cooled on ice. The reaction mixture was warmed to room temperature and stirred at 50° C. for one hour. After the reaction mixture was added with a saturated sodium bicarbonate aqueous solution and extracted with ethyl acetate while cooled on ice, the organic phase was washed with brine and dried with anhydrous magnesium sulfate. After the desiccant was filtered off, the residue obtained by evaporating the solvent under reduced pressure was purified by silica gel column chromatography-(hexane:ethyl acetate=15:1) to obtain colorless oily 4-methoxy-2-methyl-1-(4-methylbenzyl)benzene (3.89 g, 97%).

1. additionwas added dropwise
2. temperaturewhile cooled on ice
3. extractionextracted with ethyl acetate
4. temperaturewhile cooled on ice
5. washthe organic phase was washed with brine
6. dry with materialdried with anhydrous magnesium sulfate
7. filtrationAfter the desiccant was filtered off
8. customthe residue obtained
9. customby evaporating the solvent under reduced pressure
10. customwas purified by silica gel column chromatography-(hexane:ethyl acetate=15:1)