反应详情

To the methyl ester (92 mg, 0.16 mmol) of Example 373 in 3 mL of H2O/THF/acetonitrile (1:1:1) was added LiOH (16 mg, 0.65 mmol). After stirring at rt for 48 hrs, the reaction was quenched with aqueous NH4Cl (25 mL) and the product was extracted with EtOAc (60 mL). The extracts were washed with water (30 mL) and brine (30 mL), dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified on silica gel column eluting with 20-50% EtOAc in hexanes to afford the title compound. 1H NMR (500 MHz, CD3OD): δ 7.61 (1H, d), 7.46 (1H, s), 7.24 (1H, d), 7.17 (2H, d), 7.03 (1H, d), 6.93 (1H, d), 6.91 (2H, d), 1.58 (6H, s), 1.22 (9H, s). LCMS: m/e 548.2 (M+H)+.

1. customthe reaction was quenched with aqueous NH4Cl (25 mL)
2. extractionthe product was extracted with EtOAc (60 mL)
3. washThe extracts were washed with water (30 mL) and brine (30 mL)
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was purified on silica gel column
8. washeluting with 20-50% EtOAc in hexanes