反应详情

To a cooled solution (0° C.) of 17-allyl-1,14-dihydroxy-12-[2'-(4"-hydroxy-3"-methoxycyclohexyl)-1'-methylvinyl]23,25-dimethoxy-13,19,21,27-tetramethyl-11,28-dioxa-4-azatricyclo[22.3.1.04,9 ]-octacos-18-ene-2,3,10,16-tetraone (120 mg) in dry methylene chloride (15 ml) is added 2,6-lutidine (64.3 mg) followed by triisopropylsilyl trifluoromethanesulfonate (184 mg). Reaction temperature is raised to r.t. and stirred overnight under nitrogen atmosphere. The reaction is quenched with 10 ml of water and extracted with ethyl acetate. Organic layer is washed (water, sat'd NaHCO3, sat'd NaCl) and dried (anhydrous MgSO4). Removal of solvent followed by chromatography on silica gel (70% hexane/ethyl acetate) gives the title compound.

1. customReaction temperature
2. customThe reaction is quenched with 10 ml of water
3. extractionextracted with ethyl acetate
4. washOrganic layer is washed (water, sat'd NaHCO3, sat'd NaCl)
5. dry with materialdried (anhydrous MgSO4)
6. customRemoval of solvent