反应详情

A mixture of Example 36E (0.530 g, 0.792 mmol) and 5M aqueous sodium hydroxide (0.555 mL, 2.77 mmol) in dioxane (8 mL) was heated at 90° C. for 8 hours. The solvent was evaporated and the residue was treated with ethyl acetate and washed with aqueous NaHCO3. The organic layer was dried over MgSO4, filtered and concentrated until most of solvent was evaporated. The resulting precipitate was filtered, washed with ethyl acetate/ether, and vacuum oven-dried to give the title compound. The filtrate was concentrated and purified on a 4 g column using the ISCO Companion flash system eluting with ethyl acetate to give additional title compound.

1. customThe solvent was evaporated
2. additionthe residue was treated with ethyl acetate
3. washwashed with aqueous NaHCO3
4. dry with materialThe organic layer was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated until most of solvent
7. customwas evaporated
8. filtrationThe resulting precipitate was filtered
9. washwashed with ethyl acetate/ether, and vacuum
10. customoven-dried