反应详情

To a solution of INT 4 (85 mg, 0.23 mmol) in THF (2.2 mL) was added 1 M LiOH (1.1 mL, 1.14 mmol). The resulting mixture was stirred at room temperature for 19 hours. The mixture was acidified to pH 5 with 1 M HCl. The organic solvent was removed. More 1 M HCl was added to adjust the pH to 3. The mixture was extracted with EtOAc (3×). The combined organic layers were dried over MgSO4, filtered and concentrated. The residue was purified by chromatography on silica gel (CH2Cl2/MeOH) to give Example 1.

1. customThe organic solvent was removed
2. additionMore 1 M HCl was added
3. extractionThe mixture was extracted with EtOAc (3×)
4. dry with materialThe combined organic layers were dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe residue was purified by chromatography on silica gel (CH2Cl2/MeOH)
8. customto give Example 1