反应详情

To a solution of (R)-(4′-(6-chloro-2-(methylsulfonyl)-1-((2 (trimethylsilyl)ethoxy)-methyl)-1H-imidazo[4,5-b]pyridin-5-yl)-[1,1′-biphenyl]-4-yl)(3-((2-(trimethylsilyl)-ethoxy)methoxy)pyrrolidin-1-yl)methanone (150 mg, 0.198 mmol) and (4aR,7R,8aS)-2-phenylhexahydropyrano[3,2-d][1,3]dioxin-7-ol (100 mg, 0.423 mmol) in DMF (2 mL), was added cesium carbonate (150 mg, 0.460 mmol). The reaction mixture was stirred at room temperature for 2 h, then partitioned between water and EtOAc. The organic layer was separated and washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. The chromatography of the resulting residue over silica (preparative TLC) eluting with 25% EtOAc in Hexanes afforded the title compound (Rf:0.7) LC-MS: calculated for C48H61ClN4O8Si2 912.37, observed m/e: 913.6 (M+H)+ (Rt: 3.30/4 min)

1. custompartitioned between water and EtOAc
2. customThe organic layer was separated
3. washwashed with brine
4. dry with materialdried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. washThe chromatography of the resulting residue over silica (preparative TLC) eluting with 25% EtOAc in Hexanes