反应详情

Compound 66 (0.15 g, 0.158 mmol) was coevaporated with toluene (5 mL). To the residue N,N-tetraisopropylammonium tetrazolide (0.0089 g, 0.079 mmol) was added and the mixture was dried over P2O5 in a vacuum oven for overnight at 40° C. The reaction mixture was dissolved in the mixture of anhydrous acetonitrile/dichloromethane (2:1, 1 mL) and 2-cyanoethyl-N,N,N′,N′-tetraisopropylphosphorodiamidite (0.0714 g, 0.0781 mL, 0.237 mmol) was added. The reaction mixture was stirred at ambient temperature for overnight. The completion of the reaction was ascertained by TLC (1:1 ethyl acetate:hexane). The solvent was removed under reduced pressure and the residue was dissolved in ethyl acetate (10 mL) and washed with 5% NaHCO3 (4 mL) and brine (4 mL). The ethyl acetate layer was dried over anhydrous Na2SO4 and concentrated under reduced pressure. The resulting mixture was chromatographed (50:49:1, EtOAc:Hexane:triethlyamine) to afford 67 as white foam (0.152 g, 84%).

1. dry with materialthe mixture was dried over P2O5 in a vacuum oven for overnight at 40° C
2. additionwas added
3. customThe solvent was removed under reduced pressure
4. dissolutionthe residue was dissolved in ethyl acetate (10 mL)
5. washwashed with 5% NaHCO3 (4 mL) and brine (4 mL)
6. dry with materialThe ethyl acetate layer was dried over anhydrous Na2SO4
7. concentrationconcentrated under reduced pressure
8. customThe resulting mixture was chromatographed (50:49:1, EtOAc:Hexane:triethlyamine)