反应详情

Compound 4 (5 g, 21.2 mmol) and compound 5 (5.6 g, 24.3 mmol) were stirred at 0° C. CH3SO3H (50 mL) was added dropwise. Then the mixture was stirred at RT for 16 h. The reaction mixture was poured into crush ice, extracted by DCM. The DCM layer was washed with sat.Na2HPO4, dried over Na2SO4, filtered, concentrated. The residue was purified by silica gel column (DCM:EtOH=50:1), afforded compound 6 (1.2 g, 18%) as light yellow solid.

1. additionThe reaction mixture was poured
2. custominto crush ice
3. extractionextracted by DCM
4. washThe DCM layer was washed
5. dry with materialNa2HPO4, dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was purified by silica gel column (DCM:EtOH=50:1)