Reacción #470366

ord-96ecff76950647ebafe1a913cd6feca8

Ecuación de reacción

[F-].[K+]
potassium fluoride
COC[N+]1(C)CCCC1.[O-][Cl+3]([O-])([O-])[O-]
N-methoxymethyl-N-methylpyrrolidinium perchlorate
COC[N+]1(C)CCCC1.[F-]
desired product
COC[N+]1(C)CCCC1.[F-]
N-Methoxymethyl-N-Methylpyrrolidinium Fluoride

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
    workup.ADDITIONWith addition of 100 ml of methanol
  4. 4
    Filtraciónthe reaction mixture was filtered
  5. 5
    ConcentraciónThe filtrate was concentrated
  6. 6
    Otrodried in a vacuum
  7. 7
    workup.DISSOLUTIONThe residue was then dissolved in dichloromethane
  8. 8
    Filtraciónthe solution was again filtered with a membrane
  9. 9
    Filtraciónfilter
  10. 10
    Concentraciónthe filtrate was concentrated
  11. 11
    Otrodried

Procedimiento

A 0.44 g quantity of potassium fluoride (product of Wako Pure Chemical Ind. Ltd.) was dissolved in 11 g of deionized water, and 1.74 g of N-methoxymethyl-N-methylpyrrolidinium perchlorate was added to the solution. The mixture was reacted at room temperature for 1.5 hours, whereby the reaction was terminated. With addition of 100 ml of methanol, the reaction mixture was filtered. The filtrate was concentrated and dried in a vacuum. The residue was then dissolved in dichloromethane, the solution was again filtered with a membrane filter, and the filtrate was concentrated and dried, giving 1.05 g of the desired product.

Fuente

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