反应详情

To a solution of (2R,3S,5R)-5-(6-amino-9H-purin-9-yl)-2-({[tert-butyl-(dimethyl)silyl]oxy}methyl)tetrahydrofuran-3-yl acetate (2.00 g, 4.91 mmol) in CH2Br2 (98.2 mL) was added TMSBr (0.717 mL, 5.55 mmol) and t-butylnitrite (3.98 mL, 33.4 mmol). The reaction mixture was stirred at r.t. for 3 hours then slowly poured into 50 mL of a 1:1 mixture of saturated aq NaHCO3:CH2Cl2. The organic layer was washed with water (50 mL), brine (50 mL), dried (Na2SO4) and concentrated. The crude product was purified by flash chromatography (0 to 30% EtOAc/hexanes) to obtain the title compound as a yellow oil (1.26 g, 55%).

1. washThe organic layer was washed with water (50 mL), brine (50 mL)
2. dry with materialdried (Na2SO4)
3. concentrationconcentrated
4. customThe crude product was purified by flash chromatography (0 to 30% EtOAc/hexanes)