反应详情

To a suspension of the product of Step 1 in toluene (0.022 M) was added KOSiMe3 (5 equiv). The mixture was brought to reflux for 30 min, and was then stirred at room temperature overnight. Following removal of solvent under vacuum, the residue was partitioned between EtOAc/THF and H2O. The resulting emulsion was filtered, and the organic layer was dried (MgSO4), filtered, and evaporated. The crude was dissolved in TFA (0.022 M), and the resulting solution was stirred at 45° C. for 1.5 h. After removal of the TFA under vacuum, the crude material was purified by flash chromatography, eluting 1:1 EtOAc:hexanes, EtOAc, and 1:30 MeOH:EtOAc. The product was stirred with 1:10 EtOAc:hexanes containing trace acetone to give the title compound, after filtration, as an off-white solid.

1. temperatureto reflux for 30 min
2. customremoval of solvent under vacuum
3. customthe residue was partitioned between EtOAc/THF and H2O
4. filtrationThe resulting emulsion was filtered
5. dry with materialthe organic layer was dried (MgSO4)
6. filtrationfiltered
7. customevaporated
8. dissolutionThe crude was dissolved in TFA (0.022 M)
9. stirringthe resulting solution was stirred at 45° C. for 1.5 h
10. customAfter removal of the TFA under vacuum
11. customthe crude material was purified by flash chromatography
12. washeluting 1:1 EtOAc
13. stirringThe product was stirred with 1:10 EtOAc