反应详情

温度

50 °C

To a 1000 ml flask equipped with a mechanical stirrer and condenser, O-Desmethyl venlafaxine base (50 g), fumaric acid (24.24 g), and isopropyl alcohol (IPA) (1000 ml) were added at room temperature to form a mixture. The mixture was then heated to reflux. A clear solution was obtained after filtering the heated mixture through a 1-micron filter. The filtered solution was cooled to 50° C., and then gradually cooled to 5° C. over five hrs. The cooled solution was stirred at 5° C. overnight. The mixture was then heated back to 50° C., stirred at 50° C. for 2 hrs, and then cooled back to 5° C. and stirred at 5° C. for 3 hrs. A solid precipitate formed and was filtered under reduced pressure, washed with IPA, and dried in a vacuum oven, overnight, at 50° C. The obtained solid was kept in a closed container at 4° C. for five weeks, after which Form N was obtained.

1. customTo a 1000 ml flask equipped with a mechanical stirrer and condenser
2. customto form a mixture
3. temperatureThe mixture was then heated to reflux
4. customA clear solution was obtained
5. filtrationafter filtering the heated mixture through a 1-micron
6. filtrationfilter
7. temperaturegradually cooled to 5° C. over five hrs
8. temperatureThe mixture was then heated back to 50° C.
9. stirringstirred at 50° C. for 2 hrs
10. temperaturecooled back to 5° C.
11. stirringstirred at 5° C. for 3 hrs
12. customA solid precipitate formed
13. filtrationwas filtered under reduced pressure
14. washwashed with IPA
15. customdried in a vacuum oven, overnight, at 50° C
16. waitThe obtained solid was kept in a closed container at 4° C. for five weeks
17. customafter which Form N was obtained