反应详情

To a solution of ethyl (5-{3-[4-(2-bromo-5-fluorophenoxy)piperidin-1-yl]isoxazol-5-yl}-2H-tetrazol-2-yl)acetate (1.3 g, 2.62 mmol) in THF (15 mL) and MeOH (5 mL) was added 1M sodium hydroxide (5.25 mL, 5.25 mmol). The mixture was stirred at room temperature for 1 h. Volatile solvents were removed in vacuo. The residue was diluted with water (20 mL), acidified with 1M HCl (6 mL) and extracted with EtOAc. The EtOAc extract was washed with water, dried (Na2SO4) and concentrated. The residue was triturated with diethyl ether to give the crude product, containing about 5% of the 1-isomer. Further purification by trituration in isopropyl acetate (2×, 80° C. overnight, then room temperature overnight) provided the title compound as a beige powder.

1. customVolatile solvents were removed in vacuo
2. additionThe residue was diluted with water (20 mL)
3. extractionextracted with EtOAc
4. extractionThe EtOAc extract
5. washwas washed with water
6. dry with materialdried (Na2SO4)
7. concentrationconcentrated
8. customThe residue was triturated with diethyl ether
9. customto give the crude product
10. customFurther purification by trituration in isopropyl acetate (2×, 80° C. overnight