Réaction #470365

ord-067845310e5f4c2590528862f9eebda8

Équation de réaction

[Na+].[O-][Cl+3]([O-])([O-])[O-]
sodium perchlorate
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.[O-][Cl+3]([O-])([O-])[O-]
desired product
COC[N+]1(C)CCCC1.[O-][Cl+3]([O-])([O-])[O-]
N-Methoxymethyl-N-Methylpyrrolidinium Perchlorate

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    AutreThe mixture was reacted at room temperature for 1.5 hours
  2. 2
    Autrewhereby the reaction was terminated
  3. 3
    FiltrationThe resulting sodium chloride was filtered off
  4. 4
    Concentrationthe filtrate was concentrated
  5. 5
    Autredried in a vacuum
  6. 6
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane
  7. 7
    Filtrationthe solution was again filtered with a membrane
  8. 8
    Filtrationfilter
  9. 9
    Concentrationthe filtrate was concentrated in a vacuum
  10. 10
    Autredried

Mode opératoire

A 5.91 g quantity of sodium perchlorate (product of Wako Pure Chemical Ind. Ltd.) was dissolved in 77 g of ethyl alcohol, and 7.99 g of N-methoxymethyl-N-methylpyrrolidinium chloride was added to the solution. The mixture was reacted at room temperature for 1.5 hours, whereby the reaction was terminated. The resulting sodium chloride was filtered off, and the filtrate was concentrated and dried in a vacuum. The residue was dissolved in dichloromethane, the solution was again filtered with a membrane filter, and the filtrate was concentrated in a vacuum and dried, giving 10.94 g of the desired product.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08366956B2uspto-grants-2013_02