反应详情

The trisilyl derivative acid 20 (0.14 g, 0.2 mmol) was then dissolved in 5 mL dichloromethane. To the solution was added HBTU (0.19 g, 0.4 mmol), HOBt (0.076 g, 4 mmol), N-methylmorpholine (0.04 g, 0.4 mmol) and cat. DMAP. The mixture was allowed to stir at RT for 24 h. The mixture was then washed with 10% citric acid, saturated NaHCO3, brine and dried over MgSO4. The solvent was removed and the residue was treated with 5 mL 0.5N NH4F/MeOH. The solution was heated at reflux for 24 h. The solvent was evaporated and the residue was purified by preparative TLC to afford compound 21, MS 445.26 (M+1).

1. washThe mixture was then washed with 10% citric acid, saturated NaHCO3, brine
2. dry with materialdried over MgSO4
3. customThe solvent was removed
4. additionthe residue was treated with 5 mL 0.5N NH4F/MeOH
5. temperatureThe solution was heated
6. temperatureat reflux for 24 h
7. customThe solvent was evaporated
8. customthe residue was purified by preparative TLC