تفاعل #676331

ord-fabfb0f3f2a543d5ac32e0690f271c5c

معادلة التفاعل

C[N+]1(CCO)CCCC1.[Cl-]
N-hydroxyethyl-N-methylpyrrolidinium chloride
F[B-](F)(F)F.[Na+]
sodium tetrafluoroborate
ClCCl
dichloromethane
[Cl-].[Na+]
sodium chloride
C[N+]1(CCO)CCCC1.F[B-](F)(F)F
N-hydroxyethyl-N-methylpyrrolidinium tetrafluoroborate

المذيبات

ظروف التفاعل

درجة الحرارة
25°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىa pressure of about 1 atm for about 48 hours under a nitrogen atmosphere to form a mixed solution
  2. 2
    ترشيحThe mixed solution was filtered by a filter paper
  3. 3
    أخرىto remove sodium chloride
  4. 4
    أخرىto obtain a liquid
  5. 5
    workup.ADDITIONthus uniformly mixed with each other
  6. 6
    أخرىto form a mixed solution
  7. 7
    workup.WAITthe mixed solution was left at a temperature of 25° C.
  8. 8
    أخرىWhen the mixed solution was layer-separated in the separating funnel
  9. 9
    أخرىwas removed
  10. 10
    أخرىthereof was obtained
  11. 11
    أخرىto 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
    أخرىto further remove water

الإجراء التجريبي

Subsequently, about 36.9 g (0.3 mol) of the obtained N-hydroxyethyl-N-methylpyrrolidinium chloride 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 chloride. The mixed solution was filtered by a filter paper to remove sodium chloride 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 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-hydroxyethyl-N-methylpyrrolidinium tetrafluoroborate at a yield of about 65%.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09228075B2uspto-grants-2016_01