反应详情

(NH4)2SO4 (0.09 g, 0.67 mmol) was added into a stirred mixture of 8 (1.0 g, 6.61 mmol) in HMDS (20 mL, 20 P) at room temperature. The reaction mixture was then heated to reflux and maintained at that temperature for no less than 5 hours. Monitor the reaction by GC. After the reaction is completed, 14 (1.1 g, 3.77 mmol) and TMSOTf (0.29 g, 1.32 mmol) were added. Then the mixture was stirred, once the reaction was complete (as indicated by HPLC analysis) it was quenched with water (6 mL, 6 P.) and MeCN (30 mL). The mixture was filtrated and the filtrate cake was washed with MeCN (20 mL) and EtOH (5 mL), then it was dried under vacuum at 40° C. overnight to give the goal product 15 (1.92 g, 97% yield) as a yellow to brown powder with about 82.1% HPLC purity.

1. temperatureThe reaction mixture was then heated
2. temperatureto reflux
3. temperaturemaintained at that temperature for no less than 5 hours
4. customMonitor the reaction by GC
5. customwas quenched with water (6 mL, 6 P.) and MeCN (30 mL)
6. filtrationThe mixture was filtrated
7. washthe filtrate cake was washed with MeCN (20 mL) and EtOH (5 mL)
8. customit was dried under vacuum at 40° C. overnight