反应详情

温度

60 °C

To the product of EXAMPLE 61 (70 mg) in 1,4-dioxane (1 mL) was added acetic anhydride (2 mL) and DMAP (25 mg). The reaction was heated to 60° C. After about 1 hour the reaction was cooled to room temperature and quenched with methanol (1 mL) the reaction was diluted with EtOAc and 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: 590.0 (M+1), 592.0 (M+3); Rt=4.59 min.

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