反应详情

A 200 mL round bottom flask was charged with 83.18B (1.21 g, 3.21 mmol), DCM (9 mL), iodobenzene diacetate (available from Aldrich) (1.24 g, 3.86 mmol), and TEMPO (available from Aldrich) (0.0502 g, 0.321 mmol). The solution was stirred for 2 hours at room temperature and diluted with EtOAc. The organic phase was washed with saturated aqueous NaHCO3, saturated aqueous Na2S2O3, and brine, dried (MgSO4), and concentrated. The residue was purified by silica gel flash chromatography (0-5% EtOAc/hexane) to afford 83.18C (1.05 g, 87% yield) as a colorless oil.

1. washThe organic phase was washed with saturated aqueous NaHCO3, saturated aqueous Na2S2O3, and brine
2. dry with materialdried (MgSO4)
3. concentrationconcentrated
4. customThe residue was purified by silica gel flash chromatography (0-5% EtOAc/hexane)