反应详情

To the above-obtained 3-bromo-3-methylbutan-2-one (5.88 g) in methanol (30 mL), benzhydrylamine (5.0 mL) and triethylamine (7.5 mL) were added. The resultant mixture was stirred at 70° C. for 24 hours, and then cooled in air. The reaction mixture was partitioned between water and ethyl acetate. The organic layer was sequentially washed with saturated aqueous sodium hydrogencarbonate and saturated brine, and then dried over magnesium sulfate anhydrate, followed by filtration. The solvent was evaporated under reduced pressure, and to the solid, diethyl ether was added, and then insoluble matter was removed by filtration. The mother liquid was brought to the dryness under reduced pressure. The residue was purified through silica gel column chromatography (hexane-ethyl acetate), to thereby give 3-(benzhydrylamino)-3-methylbutan-2-one as an oily product (3.3 g, 34%).

1. temperaturecooled in air
2. customThe reaction mixture was partitioned between water and ethyl acetate
3. washThe organic layer was sequentially washed with saturated aqueous sodium hydrogencarbonate and saturated brine
4. dry with materialdried over magnesium sulfate anhydrate
5. filtrationfollowed by filtration
6. customThe solvent was evaporated under reduced pressure
7. additionto the solid, diethyl ether was added
8. custominsoluble matter was removed by filtration
9. customThe residue was purified through silica gel column chromatography (hexane-ethyl acetate)