反应详情

To a solution of 4-{3-methoxy-4-[5-(5-methyl-3-phenyl-isoxazol-4-yl)-[1,3,4]oxadiazol-2-yl]-phenyl}-thiomorpholine (156 mg, 0.36 mmol) in dichloromethane (2 mL) and methanol (2 mL) was added oxone (331 mg, 0.54 mmol) and the reaction mixture was stirred for 18 h at ambient temperature and then for 4 h at 50° C. After cooling to ambient temperature oxone (331 mg, 0.54 mmol) was added and stirred for 18 h at 50° C. before it was cooled to ambient temperature and sodium bisulfite solution (38%, 1.5 mL) was added and stirred for 15 min. After the addition of aqueous sodium carbonate (saturated, 10 mL) the mixture was extracted with ethyl acetate (20 mL) and washed with aqueous sodium carbonate (20 mL). After drying over sodium sulfate the concentrated residue was dissolved in dichloromethane (5 mL) and diluted with tert-butylmethylether (20 mL). The dichloromethane was distilled off and the resulting suspension was filtered affording the title compound (116 mg, 69%) as a white solid. MS: m/e=467.2 [M+H]+.

1. waitfor 4 h at 50° C
2. additionwas added
3. stirringstirred for 18 h at 50° C. before it
4. temperaturewas cooled to ambient temperature
5. stirringstirred for 15 min
6. extractionwas extracted with ethyl acetate (20 mL)
7. washwashed with aqueous sodium carbonate (20 mL)
8. dry with materialAfter drying over sodium sulfate the concentrated residue
9. dissolutionwas dissolved in dichloromethane (5 mL)
10. additiondiluted with tert-butylmethylether (20 mL)
11. distillationThe dichloromethane was distilled off
12. filtrationthe resulting suspension was filtered