Reacción #470365

ord-067845310e5f4c2590528862f9eebda8

Ecuación de reacción

[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

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe mixture was reacted at room temperature for 1.5 hours
  2. 2
    Otrowhereby the reaction was terminated
  3. 3
    FiltraciónThe resulting sodium chloride was filtered off
  4. 4
    Concentraciónthe filtrate was concentrated
  5. 5
    Otrodried in a vacuum
  6. 6
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane
  7. 7
    Filtraciónthe solution was again filtered with a membrane
  8. 8
    Filtraciónfilter
  9. 9
    Concentraciónthe filtrate was concentrated in a vacuum
  10. 10
    Otrodried

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08366956B2uspto-grants-2013_02