反应详情

温度

60 °C

To a magnetically stirred solution of 0.273 g (0.50 mmol) of the product of Example 182 in 5 mL MeOH was added 0.343 g (0.248 mmol) of potassium carbonate and 0.5 mL water. The reaction mixture was stirred at 60° C. for 3 h then cooled to room temperature and partitioned between EtOAc and 10% aq. NaHSO4. The organic extracts were separated, washed with water and brine, dried (Na2SO4), filtered and evaporated. The residue was purified on a silica gel flash chromatography column eluted with 0–20% EtOAc-hexane. Evaporation of the purified fractions and drying in vacuo afforded the titled compound. HPLC/MS: 453.9 (M+1), 455.8 (M+3); Rt=4.15 min.

1. temperaturethen cooled to room temperature
2. custompartitioned between EtOAc and 10% aq. NaHSO4
3. customThe organic extracts were separated
4. washwashed with water and brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. customevaporated
8. customThe residue was purified on a silica gel flash chromatography column
9. washeluted with 0–20% EtOAc-hexane
10. customEvaporation of the purified fractions
11. customdrying in vacuo