反应详情

A mixture of 4-Methoxy-benzenethiol (0.20 g, 1 eq) and potassium carbonate (0.47 g, 2.5 eq) in dry THF was allowed to stir at room temperature under argon for an hour. Then the stirred suspension was cooled to 0° C. and to it was added drop wise a solution of phosgene (0.17 g 1.2 eq). The reaction stirred at 0° C. for half an hour. Then 3-tert-Butyl-isoxazol-5-ylamine (0.20 g, 1 eq) in THF was added dropwise. The reaction was allowed to warm to room temperature and stirred overnight. The solvent was removed and extracted with ethyl acetate and water. The organic layer was dried over magnesium sulfate and solvent removed. It was purified by HPLC. Yield: 157 mg (36%), LC/MS [MH+] 307.

1. temperatureThen the stirred suspension was cooled to 0° C. and to it
2. stirringThe reaction stirred at 0° C. for half an hour
3. temperatureto warm to room temperature
4. stirringstirred overnight
5. customThe solvent was removed
6. extractionextracted with ethyl acetate and water
7. dry with materialThe organic layer was dried over magnesium sulfate and solvent
8. customremoved
9. customIt was purified by HPLC