反应详情

A solution of methyl 4-(1-methyl-1H-pyrazol-5-yl)-2-thiophenecarboxylate (330 mg, 1.49 mmol) and Selectfluor® (793 mg, 2.23 mmol) in THF (7 mL) and H2O (500 uL) was stirred in a sealed tube at 70° C. After 1 h, additional selectfluor (793 mg, 2.23 mmol) was added and the solution stirred an additional 12 h. The reaction mixture was then partitioned between H2O-DCM, the aqueous phase was washed several times with DCM. The combined organic fractions were dried (Na2SO4), concentrated and purified via column chromatography (silica, 20% EtOAc in hexanes) affording the title compound (126 mg, 33%) as a white solid: LCMS (ES) m/z=241 (M+H)+.

1. customThe reaction mixture was then partitioned between H2O-DCM
2. washthe aqueous phase was washed several times with DCM
3. dry with materialThe combined organic fractions were dried (Na2SO4)
4. concentrationconcentrated
5. custompurified via column chromatography (silica, 20% EtOAc in hexanes)