反应详情

温度

106 °C

A suspension of simvastatin phenylboronate (30.0 g) and 1,3-propanediol (450 mL) was heated at 105 to 107° C. at 0.2 mm Hg. After 1 hour, 182 mL of distillate was collected and the reaction was cooled to 20 to 25° C. Deionized water (270 mL) was added and toluene (3×75 mL) was used to extract the mixture. The combined toluene layers were washed with water (2×30 mL). The organic solution was heated at reflux for 1 hour and water was azeotropically removed. The solution was concentrated to a final volume of 24 mL under vacuum at 48 to 50° C. To the concentrated solution was added hexanes (215 mL) over 10 minutes. The resulting slurry was cooled to 0 to 5° C. and filtered. The crude simvastatin was washed with 0 to 5° C. hexanes and dried under vacuum to yield 21.0 g (88%) of simvastatin.

1. distillation182 mL of distillate was collected
2. temperaturethe reaction was cooled to 20 to 25° C
3. additionDeionized water (270 mL) was added
4. extractionto extract the mixture
5. washThe combined toluene layers were washed with water (2×30 mL)
6. temperatureThe organic solution was heated
7. temperatureat reflux for 1 hour
8. customwater was azeotropically removed
9. concentrationThe solution was concentrated to a final volume of 24 mL under vacuum at 48 to 50° C
10. additionTo the concentrated solution was added hexanes (215 mL) over 10 minutes
11. temperatureThe resulting slurry was cooled to 0 to 5° C.
12. filtrationfiltered
13. washThe crude simvastatin was washed with 0 to 5° C. hexanes
14. customdried under vacuum