反应详情

温度

-78 °C

To a solution of 66.30B (0.400 g, 0.925 mmol) in toluene (10 mL) at −78° C. was added DAST (0.209 g, 1.29 mmol) dropwise. The reaction was stirred at −78° C. for 30 minutes and then warmed to 23° C. and stirred for an additional 2 hours. Water was added to quench the reaction mixture. The reaction was then extracted three times with EtOAc. After drying over anhydrous magnesium sulfate and filtering, the organic solvent was removed under reduced pressure and the product was then purified on silica gel (0-10% EtOAc in hexanes) to yield 66.30C as a colorless oil (0.400 g, 99% yield).

1. temperaturewarmed to 23° C.
2. stirringstirred for an additional 2 hours
3. customto quench the reaction mixture
4. extractionThe reaction was then extracted three times with EtOAc
5. dry with materialAfter drying over anhydrous magnesium sulfate
6. filtrationfiltering
7. customthe organic solvent was removed under reduced pressure
8. customthe product was then purified on silica gel (0-10% EtOAc in hexanes)