反应详情

温度

50 °C

1-(2-Chlorophenyl)ethyl[3-(4-chloromethylphenyl)-4-isoxazolyl]carbamate (1.0 g, 2.56 mmol) obtained in Step B-6 of Example 1 was dissolved in N,N-dimethylformamide (30 ml), methyl 3-aminopropionate hydrochloride (1.07 g, 7.67 mmol) and potassium carbonate (2.12 g, 15.3 mmol) were added, and the mixture was stirred overnight at 50° C. 1N Hydrochloric acid was added at 0° C. to weak-acidify the reaction system, and the mixture was extracted 3 times with ethyl acetate. The organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and saturated aqueous sodium chloride solution, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by column chromatography (methanol:dichloromethane=1:20) to give the title compound (138 mg, 11%).

1. extractionthe mixture was extracted 3 times with ethyl acetate
2. washThe organic layer was washed with saturated aqueous sodium hydrogencarbonate solution and saturated aqueous sodium chloride solution
3. dry with materialdried over anhydrous sodium sulfate
4. customThe solvent was evaporated under reduced pressure
5. customthe residue was purified by column chromatography (methanol:dichloromethane=1:20)