反应详情

To a solution of methanone 167 (7.9 g, 22.6 mmol) in TFA (90 mL) were added triethylsilane (18.5 mL, 113 mmol) and catalytic triflic acid at 0° C. The mixture was warmed up to room temperature slowly and stirred at room temperature for 15 hours. The mixture was evaporated in vacuo. The residue was diluted with EtOAc (150 mL) and neutralized with aq. Saturated NaHCO3 solution. The mixture was extracted with EtOAc (150 mL×1). The organic layer was dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by silica gel column chromatography to provide the compound 168 (6.1 g, 80.1%).

1. customThe mixture was evaporated in vacuo
2. additionThe residue was diluted with EtOAc (150 mL)
3. extractionThe mixture was extracted with EtOAc (150 mL×1)
4. dry with materialThe organic layer was dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was purified by silica gel column chromatography