Reaktion #470364

ord-143614ae0ca4455dacc462476a3cf9db

Reaktionsgleichung

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

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe mixture was reacted at room temperature for 0.5 hour
  2. 2
    Sonstigewhereby the reaction was terminated
  3. 3
    EinengenThe reaction mixture was concentrated
  4. 4
    Trocknendried in vacuum, and 100 ml of ethyl alcohol
  5. 5
    workup.ADDITIONwas added to the residue
  6. 6
    Sonstigeto 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
    Einengenthe filtrate was concentrated in a vacuum
  11. 11
    Sonstigedried

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08366956B2uspto-grants-2013_02