تفاعل #470365

ord-067845310e5f4c2590528862f9eebda8

معادلة التفاعل

[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

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىThe mixture was reacted at room temperature for 1.5 hours
  2. 2
    أخرىwhereby the reaction was terminated
  3. 3
    ترشيحThe resulting sodium chloride was filtered off
  4. 4
    تركيزthe filtrate was concentrated
  5. 5
    أخرىdried in a vacuum
  6. 6
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane
  7. 7
    ترشيحthe solution was again filtered with a membrane
  8. 8
    ترشيحfilter
  9. 9
    تركيزthe filtrate was concentrated in a vacuum
  10. 10
    أخرىdried

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08366956B2uspto-grants-2013_02