反应详情

To a solution of 73B (2.34 g, 10.9 mmol) in 30 mL DMF, was added imidazole (1.11 g, 16.3 mmol) and tert-butyldimethylsilyl chloride (1.97 g, 13.1 mmol). The mixture was stirred at rt for 3 h, then was diluted with hexanes. The organic phase washed with H2O (2×) and brine, dried (Na2SO4) and concentrated. The product was purified by flash chromatography (0 to 10% EtOAc/hexanes gradient) to afford 2.00 g of 73C as a colorless oil. MS (ESI) m/z 197.1 (M-OTBS)+.

1. washThe organic phase washed with H2O (2×) and brine
2. dry with materialdried (Na2SO4)
3. concentrationconcentrated
4. customThe product was purified by flash chromatography (0 to 10% EtOAc/hexanes gradient)