反应详情

A solution of 2.2 g of potassium t-butoxide (19.9 mmol) in tetrahydrofuran (130 ml) was added to a solution of 5.8 g of {2-[(2-bromoacetyl)-(2-chloro-5-fluorophenyl)amino]-1,1-dimethylethyl}carbamic acid t-butyl ester obtained in Example (62b) (13.3 mmol) in tetrahydrofuran (130 ml) under a nitrogen atmosphere and under cooling in a dry ice-acetone bath over 30 minutes, and the mixture was stirred at the same temperature for 10 minutes. A saturated ammonium chloride aqueous solution was added to the reaction mixture. The mixture was returned to room temperature and diluted with water, followed by extraction with ethyl acetate. Then, 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:methylene chloride/ethyl acetate=10/1) to obtain 2.79 g of the title compound (yield: 64%).

1. temperatureunder cooling in a dry ice-acetone bath over 30 minutes
2. customwas returned to room temperature
3. extractionfollowed by extraction with ethyl acetate
4. dry with materialThen, the organic layer was dried over anhydrous magnesium sulfate
5. filtrationAfter filtration
6. customthe solvent was evaporated under reduced pressure
7. customthe residue was purified by silica gel column chromatography (elution solvent:methylene chloride/ethyl acetate=10/1)