反应详情

A mixture of ethyl 5-(2,4-bis(benzyloxy)-5-chlorophenyl)isoxazole-3-carboxylate (200 mg, 0.43 mmol), methanol (10 ml), water (6-7 ml), and LiOH (16 mg, 0.65 mmol) was allowed to stand at 50-60° C. for 24 h. The solution was concentrated under vacuo to remove methanol, and the remaining aqueous solution was extracted with Et2O to remove traces of unreacted starting material. The aqueous solution was acidified with 1 M HCl and extracted with three portions of AcOEt. The combined organic extracts were washed with saturated aqueous sodium chloride and dried over sodium sulfate. Removal of the solvent under reduced pressure afforded a residue, which was chromatographed on silica gel (DCM/methanol: 9/1).

1. concentrationThe solution was concentrated under vacuo
2. customto remove methanol
3. extractionthe remaining aqueous solution was extracted with Et2O
4. customto remove traces
5. extractionextracted with three portions of AcOEt
6. washThe combined organic extracts were washed with saturated aqueous sodium chloride
7. dry with materialdried over sodium sulfate
8. customRemoval of the solvent under reduced pressure
9. customafforded a residue, which
10. customwas chromatographed on silica gel (DCM/methanol: 9/1)