反应详情

To a solution of 1A (2.7 g, 10.9 mmol) in THF (50 mL) at RT was added dropwise a solution of pyridinium tribromide (3.83 g, 0.41 mmol) in THF (50 mL). After addition, the reaction mixture was stirred for 15 min, then water (60 mL) and ether (60 mL) added. The aqueous layer was separated, and extracted with EtOAc (2×50 mL). The combined organics were washed with brine, dried (Na2SO4) and concentrated. The residue was chromatographed (silica gel) eluting with EtOAc (0 to 50%) in hexane to give the title compound (2.5 g, 70% yield) as a white solid.

1. additionAfter addition
2. customThe aqueous layer was separated
3. extractionextracted with EtOAc (2×50 mL)
4. washThe combined organics were washed with brine
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customThe residue was chromatographed (silica gel)
8. washeluting with EtOAc (0 to 50%) in hexane