反应详情

温度

0 °C

To a solution of [3-(5-fluoro-pyridin-2-yl)-5-methyl-isoxazol-4-yl]-methanol (1.9 g, 9.13 mmol) in DCM (38 mL) was added a suspension of DMP (4.65 g, 10.96 mmol) in DCM (30 mL) portionwise and under argon at room temperature and then the mixture was cooled to 0° C. and the resulting mixture warmed up to room temperature overnight. The mixture was then poured carefully into stirred saturated sodium hydrogen carbonate solution and the aqueous layer extracted with DCM. The combined organic layers were then washed with brine, dried over sodium sulfate and evaporated. Purification by chromatography (silica, 0 to 50% ethyl acetate in heptane) gave the title compound (1.7 g, 90%) as a white solid. MS: m/e=207.0 [M+H]+. Alternatively

1. temperaturethe resulting mixture warmed up to room temperature overnight
2. additionThe mixture was then poured carefully
3. extractionthe aqueous layer extracted with DCM
4. washThe combined organic layers were then washed with brine
5. dry with materialdried over sodium sulfate
6. customevaporated
7. customPurification by chromatography (silica, 0 to 50% ethyl acetate in heptane)