反应详情

1.08 g of sodium bicarbonate (12.9 mmol) and 1.0 ml of bromoacetyl bromide (11.3 mmol) were added to a solution of 4.00 g of [2-(2-benzyloxyphenylamino)-1,1-dimethylethyl]carbamic acid t-butyl ester obtained in Example (10a) (10.7 mmol) in a mixed solvent of ethyl acetate (50 ml) and water (50 ml) under ice-cooling, and the mixture was stirred at the same temperature for 10 minutes. After extraction with ethyl acetate, the organic layer was dried over anhydrous magnesium sulfate. After filtration, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography (elution solvent:hexane/ethyl acetate=2/1) to obtain 4.86 g of the title compound (yield: 92%).

1. temperaturecooling
2. extractionAfter extraction with ethyl acetate
3. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
4. filtrationAfter filtration
5. customthe solvent was evaporated under reduced pressure
6. customthe residue was purified by silica gel column chromatography (elution solvent:hexane/ethyl acetate=2/1)