反应详情

TBDPSCl (3.5 g, 12.6 mmol, 1.1 equiv) and imidazole (1.95 g, 28.7 mmol, 2.5 equiv) were added to a solution of 2.21.1b (3.8 g, 11.4 mmol, 1.0 equiv) in DMF (11.5 mL) at room temperature and the mixture was stirred at room temperature for 1 hour. The mixture was diluted with EtOAc and washed with saturated aqueous NH4Cl solution, brine, dried over Na2SO4 and concentrated. The residue was purified by silica gel column chromatography (EtOAc/heptane, 0 to 50%) to give product 5.4 g (83% yield). MS m/z (M+Na) 592

1. washwashed with saturated aqueous NH4Cl solution, brine
2. dry with materialdried over Na2SO4
3. concentrationconcentrated
4. customThe residue was purified by silica gel column chromatography (EtOAc/heptane, 0 to 50%)