Sodium Chloride → HCID 86660713, compound

HRID 1852300Notes

Reaction equation

HRID 1852300 reaction equation
[Cl-].[OH:2][CH2:3][CH2:4][N+:5]1([CH3:10])[CH2:9][CH2:8][CH2:7][CH2:6]1.[F:11][B-:12]([F:15])([F:14])[F:13].[Na+].[Cl-].[Na+].ClCCl>CC(C)=O.O>[F:11][B-:12]([F:15])([F:14])[F:13].[OH:2][CH2:3][CH2:4][N+:5]1([CH3:10])[CH2:9][CH2:8][CH2:7][CH2:6]1

Participants

7

Reactant 4

HCID 5234Sodium ChlorideHCID 6344DichloromethaneHCID 4343483Sodium TetrafluoroborateHCID 67996924HCID 67996924, compound

Product 1

HCID 86660713HCID 86660713, compound

Reagents, catalysts & solvents 2

HCID 180AcetoneSolventHCID 962WaterSolvent

Conditions

Temperature
25 °C

Procedure

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%.

Workup

  1. customa pressure of about 1 atm for about 48 hours under a nitrogen atmosphere to form a mixed solution
  2. filtrationThe mixed solution was filtered by a filter paper
  3. customto remove sodium chloride
  4. customto obtain a liquid
  5. additionthus uniformly mixed with each other
  6. customto form a mixed solution
  7. waitthe mixed solution was left at a temperature of 25° C.
  8. customWhen the mixed solution was layer-separated in the separating funnel
  9. customwas removed
  10. customthereof was obtained
  11. customto obtain a final liquid
  12. waitThe final liquid was left in a vacuum oven at about 35° C. for about 48 hours
  13. customto further remove water

Sources & evidence

ORD record
ord-0ff83e50f84546c0b39dcdcd92a01574
Source dataset
uspto-grants-2015_02
Patent number
US08961656B2

Reaction notes

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