反应详情

A solution of (2) (2.26 g, 8.97 mmol) and tetrabutylammonium fluoride (1 M in tetrahydrofuran, 36 mL, 36 mmol) in tetrahydrofuran was stirred at room temperature under argon for 3 hours. Dichloromethane (100 mL) and water (150 mL) were added. The organic layer was separated and the aqueous layer was extracted with dichloromethane (3×15 mL). The combined organic layers were washed with brine (200 mL), dried over anhydrous magnesium sulfate, filtered and the solvent completely removed. The residue was purified by passing through a silica plug using dichloromethane as eluent to give (3) (1.44 g, 90%).

1. customThe organic layer was separated
2. extractionthe aqueous layer was extracted with dichloromethane (3×15 mL)
3. washThe combined organic layers were washed with brine (200 mL)
4. dry with materialdried over anhydrous magnesium sulfate
5. filtrationfiltered
6. customthe solvent completely removed
7. customThe residue was purified