反应详情

To DAST (0.15 mL, 1.1 mmol) in anhydrous CHCl3 (0.6 mL) at -78° C. is slowly added compound 9 (536 mg, 1.0 mmol) in CHCl3 (2.0 mL). After 10 minutes, the reaction mixture is warmed to ambient temperature and stirred (20 minutes). The mixture is slowly diluted with brine (10 mL) then extracted with CHCl3 (2×10 mL) and the combined extracts dried (MgSO4) and evaporated under reduced pressure to yield crude 20 (629 mg). Purification by silica gel chromatography affords pure 20 as a syrup (295 mg, 55%).

1. customat -78° C.
2. extractionthen extracted with CHCl3 (2×10 mL)
3. dry with materialthe combined extracts dried (MgSO4)
4. customevaporated under reduced pressure