Реакция #470365

ord-067845310e5f4c2590528862f9eebda8

Уравнение реакции

[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

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
    ФильтрацияThe resulting sodium chloride was filtered off
  4. 4
    Концентрированиеthe filtrate was concentrated
  5. 5
    Другоеdried in a vacuum
  6. 6
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane
  7. 7
    Фильтрацияthe solution was again filtered with a membrane
  8. 8
    Фильтрацияfilter
  9. 9
    Концентрированиеthe filtrate was concentrated in a vacuum
  10. 10
    Другоеdried

Методика

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.

Источник

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