反应详情

温度

58 °C

Crude CCI-779 boronate (300 g) and acetone (900 g) was charged into a flask. The mixture was heated to reflux (55 to 61° C.) and held for 1 h. The mixture was cooled to 20-25° C. over 2-3 h, then distilled to remove acetone under vacuum (23-26″ Hg) at a pot temperature not exceeding 10-18° C. (final volume 940-960 mL). The diethyl ether (450 g) was added, stirred at 18-25° C. for 18 hours, and then filtered to give crude CCI-779 boronate (225 g, LOD=0.95%). The filtered crude CCI-779 boronate (224 g) and acetone (676 g) was charged into a flask. The mixture was heated to reflux (55 to 61° C.) and held for 1 h. The mixture was cooled to 19-25° C. over 2-3 h, then distilled to remove acetone under vacuum (18-20″ Hg) at a pot temperature of 18-20° C. (final volume 620 mL). The diethyl ether (338 g) was added, stirred at 18-25° C. for 18 hours, and then filtered. After washing 3 times using ether (250 mL each) to give CCI-779 boronate in 63% yield (LOD=0.57%, strength=85.9%, total impurities=1.8%, LSI=0.50, rapamycin=0.95%).

1. temperatureThe mixture was heated
2. temperatureThe mixture was cooled to 20-25° C. over 2-3 h
3. distillationdistilled
4. customto remove acetone under vacuum (23-26″ Hg) at a pot temperature not
5. customexceeding 10-18° C.
6. additionThe diethyl ether (450 g) was added
7. filtrationfiltered
8. customto give crude CCI-779 boronate (225 g, LOD=0.95%)
9. filtrationThe filtered crude CCI-779 boronate (224 g) and acetone (676 g)
10. additionwas charged into a flask
11. temperatureThe mixture was heated
12. temperatureto reflux (55 to 61° C.)
13. waitheld for 1 h
14. temperatureThe mixture was cooled to 19-25° C. over 2-3 h
15. distillationdistilled
16. customto remove acetone under vacuum (18-20″ Hg) at a pot temperature of 18-20° C. (final volume 620 mL)
17. additionThe diethyl ether (338 g) was added
18. stirringstirred at 18-25° C. for 18 hours
19. filtrationfiltered
20. washAfter washing 3 times