反应详情

温度

25 °C

The title compound from Step A above (4.61 g) (7.5 mmoles) was dissolved in methanol (40 mL) and a 10% (v/v) conc. H2SO4 in dioxane solution (100 mL) was added. The mixture was stirred at 25° C. for 2 h and then basified with conc. aqueous NaOH. The mixture was extracted with dichloromethane and the latter was washed with water, dried over MgSO4, filtered and evaporated to dryness. The product was chromatographed on silica gel using 10% (10% conc. NH4OH in methanol)dichloromethane as the eluant to give the title compound (Yield: 2.86 g; 74%)

1. extractionThe mixture was extracted with dichloromethane
2. washthe latter was washed with water
3. dry with materialdried over MgSO4
4. filtrationfiltered
5. customevaporated to dryness
6. customThe product was chromatographed on silica gel using 10% (10% conc. NH4OH in methanol)dichloromethane as the eluant