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温度

0 °C

A suspension of 3-[4-(2-trifluoromethylsulfanyl-benzyloxy)-phenyl]-isoxazole-5-carboxylic acid amide (which may be prepared as described in Example 1; 60 mg, 0.153 mmol) in CH2Cl2 (8 mL) was cooled to 0° C. in an ice-water bath. MCPBA (130 mg, 5 equivalents) was added and the mixture was stirred at 0° C. for 1 h and then at room temperature overnight. The reaction mixture was washed with 10% aqueous Na2SO3 and saturated aqueous NaHCO3, dried (Na2SO4), filtered, evaporated and purified by chromatography (35-45% EtOAc/hexanes) to give 3-[4-(2-trifluoromethanesulfinyl-benzyloxy)-phenyl]-isoxazole-5-carboxylic acid amide (16.2 mg, 26%) as a white solid. HRMS Calcd. for C18H14F3N2O4S (M+H)+, 411.0621. Found: 411.0617.

1. customat room temperature
2. customovernight
3. washThe reaction mixture was washed with 10% aqueous Na2SO3 and saturated aqueous NaHCO3
4. dry with materialdried (Na2SO4)
5. filtrationfiltered
6. customevaporated
7. custompurified by chromatography (35-45% EtOAc/hexanes)