반응 #470365

ord-067845310e5f4c2590528862f9eebda8

반응 방정식

[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

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The mixture was reacted at room temperature for 1.5 hours
  2. 2
    기타whereby the reaction was terminated
  3. 3
    여과The resulting sodium chloride was filtered off
  4. 4
    농축the filtrate was concentrated
  5. 5
    기타dried in a vacuum
  6. 6
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane
  7. 7
    여과the solution was again filtered with a membrane
  8. 8
    여과filter
  9. 9
    농축the filtrate was concentrated in a vacuum
  10. 10
    기타dried

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08366956B2uspto-grants-2013_02