Réaction #490256

ord-f4a1b606eae64693adceefd212067b61

Équation de réaction

O=C([O-])[O-].[Na+].[Na+]
sodium carbonate
COC[N+]1(C)CCCC1.[Cl-]
N-methoxymethyl-N-methylpyrrolidinium chloride
COC[N+]1(C)CCCC1.[Cl-]
N-methyl-N-methoxymethylpyrrolidinium chloride
COC[N+]1(C)CCCC1.COC[N+]1(C)CCCC1.O=C([O-])[O-]
desired product
COC[N+]1(C)CCCC1.COC[N+]1(C)CCCC1.O=C([O-])[O-]
N-methoxymethyl-N-methylpyrrolidinium carbonate

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreThe mixture was reacted at room temperature for 0.5 hour
  2. 2
    Autrewhereby the reaction was terminated
  3. 3
    ConcentrationThe reaction mixture was concentrated
  4. 4
    Séchagedried in vacuum, and 100 ml of ethyl alcohol
  5. 5
    workup.ADDITIONwas added to the residue
  6. 6
    Autreto remove insoluble sodium chloride
  7. 7
    workup.DISSOLUTIONThe resulting product was dissolved in dichloromethane
  8. 8
    Filtrationthe solution was filtered with a membrane
  9. 9
    Filtrationfilter again
  10. 10
    Concentrationthe filtrate was concentrated in a vacuum
  11. 11
    Autredried

Mode opératoire

A 1.60 g quantity of sodium carbonate (product of Wako Pure Chemical Ind. Ltd.) was dissolved in 18 g of deionized water, and 5.01 g of N-methoxymethyl-N-methylpyrrolidinium chloride was added to the solution. The mixture was reacted at room temperature for 0.5 hour, whereby the reaction was terminated. The reaction mixture was concentrated and dried in vacuum, and 100 ml of ethyl alcohol was added to the residue to remove insoluble sodium chloride. The resulting product was dissolved in dichloromethane, the solution was filtered with a membrane filter again, and the filtrate was concentrated in a vacuum and dried, giving 5.41 g of the desired product.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08747690B2uspto-grants-2014_06