反应详情

温度

105 °C

To the product of EXAMPLE 72 (48.8 mg) in 1,4-dioxane (1 mL) was added acetic anhydride (2 mL) and DMAP (20 mg). The reaction was heated to 105° C. After about 1 hour the reaction was cooled to room temperature and diluted with EtOAc. The solution washed with saturated aqueous NaHCO3/1 M aqueous NaOH solution (1:1). The organic layer was dried (Na2SO4). The concentrated residue was purified by flash chromatography on silica gel gradient eluted with 0-100% EtOAc in hexane affording the title compound. HPLC/MS: 557.1 (M+1), 559.1 (M+3); Rt=4.40 min.

1. temperatureAfter about 1 hour the reaction was cooled to room temperature
2. washThe solution washed with saturated aqueous NaHCO3/1 M aqueous NaOH solution (1:1)
3. dry with materialThe organic layer was dried (Na2SO4)
4. customThe concentrated residue was purified by flash chromatography on silica gel gradient
5. washeluted with 0-100% EtOAc in hexane affording the title compound