反应详情

To 2-b′ (9 g, 25 mmol), diethyl phosphite (10.5 g, 75 mmol) and Et3N (8.5 g, 75 mmol) in toluene was added PdCl2(dppf) (7.5 g). The mixture was allowed to stir overnight at reflux. The mixture was filtered and the filtrate was concentrated under vacuum. The residue was taken into ethyl acetate and washed with saturated NH3Cl. The organic layer was concentrated under vacuum and the residue was purified over silica gel to provide the crude product 2-c (15 g). (M+Na)+=442.

1. temperatureat reflux
2. filtrationThe mixture was filtered
3. concentrationthe filtrate was concentrated under vacuum
4. washwashed with saturated NH3Cl
5. concentrationThe organic layer was concentrated under vacuum
6. customthe residue was purified over silica gel