Реакция #470366

ord-96ecff76950647ebafe1a913cd6feca8

Уравнение реакции

[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

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe mixture was reacted at room temperature for 1.5 hours
  2. 2
    Другоеwhereby the reaction was terminated
  3. 3
    workup.ADDITIONWith addition of 100 ml of methanol
  4. 4
    Фильтрацияthe reaction mixture was filtered
  5. 5
    КонцентрированиеThe filtrate was concentrated
  6. 6
    Другоеdried in a vacuum
  7. 7
    workup.DISSOLUTIONThe residue was then dissolved in dichloromethane
  8. 8
    Фильтрацияthe solution was again filtered with a membrane
  9. 9
    Фильтрацияfilter
  10. 10
    Концентрированиеthe filtrate was concentrated
  11. 11
    Другоеdried

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08366956B2uspto-grants-2013_02