Réaction #1699046

ord-cf5f4edbce414ac4b2dc7c3180ad2dd6

Équation de réaction

CCCC[n+]1ccn(C)c1.[Cl-]
1-butyl-3-methylimidazolium chloride
O=[N+]([O-])O
HNO3
O=[N+]([O-])O
nitric acid
CCCC[n+]1ccn(C)c1.O=[N+]([O-])[O-]
1-butyl-3-methylimidazolium nitrate
Rendement 51.0%

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    workup.ADDITIONwas added to the third compartment
  2. 2
    workup.ADDITIONcontaining solution
  3. 3
    Autrethe second solution was removed from the cell
  4. 4
    workup.ADDITION85% BMIM Chloride was added continuously to the first compartment
  5. 5
    Températureto maintain a concentration of 2 M in that compartment during the electrolysis
  6. 6
    Autreto remove residual nitric acid
  7. 7
    Autreevaporated under rotary vacuum

Mode opératoire

In a third example, a three-compartment cell was constructed using a anode, a cation exchange membrane, an anion exchange membrane, and a cathode. 3 Liters of a 2 M solution of 1-butyl-3-methylimidazolium chloride was added to the first compartment, and 3 liters of a 3 M solution of HNO3 was added to the second compartment, and 0.5 liters of 1 M KOH was added to the third compartment. Electricity was applied to the cell, until the pH of the nitric acid-containing solution had risen to 7.0, whereupon the electrolysis was stopped and the second solution was removed from the cell. 85% BMIM Chloride was added continuously to the first compartment to maintain a concentration of 2 M in that compartment during the electrolysis. The second solution was passed through a weakbase ion exchange resin to remove residual nitric acid, then evaporated under rotary vacuum. The product, 1-butyl-3-methylimidazolium nitrate was obtained in 51% yield and contained 418 ppm potassium, 852 ppm chloride,and 3.24% water.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US06991718B2uspto-grants-2006_01