反应详情

Thiophene-2-sulfonyl chloride (183 mg, 1 mmol) was added to a solution of 3-amino-4-bromo-5-methylisoxazole (177 mg, 1 mmol) in dry pyridine (0.5 ml). The reaction mixture was stirred at room temperature for 3 h. Pyridine was removed under reduced pressure and the residue was partitioned between water and ethyl acetate. The organic layer was washed with 1N HCl (3×10 ml), brine (10 ml) and dried over anhydrous magnesium sulfate. Evaporation of the solvents left an oily residue which was solidified at -20° C. and then purified by recrystallization from ethyl acetate/hexanes, to give the pure product (51% yield) as a tan solid, m.p. 156°-158° C.

1. customPyridine was removed under reduced pressure
2. customthe residue was partitioned between water and ethyl acetate
3. washThe organic layer was washed with 1N HCl (3×10 ml), brine (10 ml)
4. dry with materialdried over anhydrous magnesium sulfate
5. customEvaporation of the solvents
6. waitleft an oily residue which
7. customwas solidified at -20° C.
8. custompurified by recrystallization from ethyl acetate/hexanes