反应详情

To a mixture of di-tert-butyl{3-[3-(hydroxymethyl)isoxazol-5-yl]pyridin-2-yl}imidodicarbonate (0.78 g, 2 mmol), triethylamine (1.95 mL, 14 mmol) and 1,2-dimethoxyethane (10 mL) was added phosphorus tribromide (0.37 mL, 4 mmol) dropwise at 0° C., which was stirred at room temperature for two hours, and then stirred at 50° C. for 30 minutes. The reaction mixture was cooled to 0° C., then water was added thereto and extracted with ethyl acetate, and the organic layer was washed with saturated sodium chloride water. After drying over anhydrous magnesium sulfate and filtering, the solvent was evaporated under a reduced pressure, the residue was purified by silica gel column chromatography to obtain the title compound (0.14 g).

1. stirringstirred at 50° C. for 30 minutes
2. temperatureThe reaction mixture was cooled to 0° C.
3. extractionextracted with ethyl acetate
4. washthe organic layer was washed with saturated sodium chloride water
5. dry with materialAfter drying over anhydrous magnesium sulfate
6. filtrationfiltering
7. customthe solvent was evaporated under a reduced pressure
8. customthe residue was purified by silica gel column chromatography