反应详情

4-Hydroxy-4-(6-methoxy-pyridin-3-yl)-cyclohexanone (as prepared in the previous step, 750 mg, 3.40 mmol) in THF (5 mL) was treated with Burgess' reagent (Aldrich, 1.19 g, 5.0 mmol) at room temperature. The reaction was stirred for 10 hours. The solvent was removed in vacuo and the residue was partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over anhydrous Na2SO4, filtered and concentrated to give yellow oil, which was then purified by silica gel column on a CombiFlash® system using hexanes and ethyl acetate (from 10% ethyl acetate to 100% ethyl acetate) to afford the title compound as white solid.

1. customThe solvent was removed in vacuo
2. customthe residue was partitioned between ethyl acetate and water
3. washThe organic layer was washed with brine
4. dry with materialdried over anhydrous Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customto give yellow oil, which
8. customwas then purified by silica gel column on a CombiFlash® system