反应详情

To a solution of compound 3A (0.591 g, 2.27 mmol) in CH2Cl2 (6.5 mL) at rt was added imidazole (0.464 g, 6.81 mmol) followed by tert-butydimethylsilyl chloride (1.71 g, 11.4 mmol). After stirring overnight, the reaction mixture was partitioned between H2O and CH2Cl2. The CH2Cl2 layer was washed with 1 M H3PO4 and water, then dried (MgSO4), filtered and concentrated under reduced pressure. The residue was chromatographed (silica gel) eluting with 30% EtOAc/hexane to yield compound 3B (0.519 g). LC/MS m/z 396 [M+Na]+.

1. customthe reaction mixture was partitioned between H2O and CH2Cl2
2. washThe CH2Cl2 layer was washed with 1 M H3PO4 and water
3. dry with materialdried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customThe residue was chromatographed (silica gel)
7. washeluting with 30% EtOAc/hexane