反应详情

To a solution of [3-(5-fluoro-pyridin-2-yl)-5-methyl-isoxazol-4-yl]-methanol (2.10 g, 10.1 mmol) in DCM (240 mL) was added manganese(IV) oxide (activated 85%, 20.63 g, 201 mmol) and the reaction mixture was stirred vigorously at room temperature for 3 days. The reaction mixture was filtered through dicalite and then fresh manganese(IV) oxide (activated 85%, 20.63 g, 201 mmol) was added and the reaction mixture stirred vigorously at room temperature for another 4 days. The reaction mixture was filtered through dicalite and evaporated. The combined DCM extracts were then dried over sodium sulfate, filtered and evaporated. Purification by chromatography (silica, 0 to 50% ethyl acetate in heptane) gave the title compound (845 mg, 40%) as a white solid. MS: m/e=207.0 [M+H]+.

1. filtrationThe reaction mixture was filtered through dicalite
2. stirringthe reaction mixture stirred vigorously at room temperature for another 4 days
3. filtrationThe reaction mixture was filtered through dicalite
4. customevaporated
5. dry with materialThe combined DCM extracts were then dried over sodium sulfate
6. filtrationfiltered
7. customevaporated
8. customPurification by chromatography (silica, 0 to 50% ethyl acetate in heptane)