Reaktion #676333

Reaktionsgleichung

N-butyl-N-methylpyrrolidinium bromide

sodium tetrafluoroborate

dichloromethane

sodium bromide

→

N-butyl-N-methylpyrrolidinium tetrafluoroborate

Lösungsmittel

acetone

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigea pressure of about 1 atm for about 48 hours under a nitrogen atmosphere to form a mixed solution
2. 2
   FiltrationThe mixed solution was filtered by a filter paper
3. 3
   Sonstigeto remove sodium bromide
4. 4
   Sonstigeto obtain a liquid
5. 5
   workup.ADDITIONthus uniformly mixed with each other
6. 6
   Sonstigeto form a mixed solution
7. 7
   workup.WAITthe mixed solution was left at a temperature of about 25° C.
8. 8
   SonstigeWhen the mixed solution was layer-separated in the separating funnel
9. 9
   Sonstigewas removed
10. 10
    Sonstigethereof was obtained
11. 11
    Sonstigeto obtain a final liquid
12. 12
    workup.WAITThe final liquid was left in a vacuum oven at about 35° C. for about 48 hours
13. 13
    Sonstigeto further remove water

Vorschrift

Subsequently, about 24.8 g (0.3 mol) of the obtained N-butyl-N-methylpyrrolidinium bromide and about 32.3 g (0.3 mol) of sodium tetrafluoroborate were dissolved in about 200 mL of acetone, and were then stirred at a temperature of about 25° C. and a pressure of about 1 atm for about 48 hours under a nitrogen atmosphere to form a mixed solution containing sodium bromide. The mixed solution was filtered by a filter paper to remove sodium bromide therefrom to obtain a liquid. Then, the obtained liquid, about 50 mL of dichloromethane, and about 0.5 mL of distilled water were shaken in a separating funnel for about 10 minutes and thus uniformly mixed with each other to form a mixed solution, and then the mixed solution was left at a temperature of about 25° C. and a pressure of about 1 atm for about 48 hours. When the mixed solution was layer-separated in the separating funnel according to a density, the liquid located in a lower portion of the separating funnel was removed, and the liquid located in an upper portion thereof was obtained. These processes were repeatedly conducted three times to obtain a final liquid. The final liquid was left in a vacuum oven at about 35° C. for about 48 hours to further remove water therefrom, thereby obtaining N-butyl-N-methylpyrrolidinium tetrafluoroborate at a yield of about 45%.

Quelle