反応 #470365

ord-067845310e5f4c2590528862f9eebda8

反応方程式

[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

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The mixture was reacted at room temperature for 1.5 hours
  2. 2
    その他whereby the reaction was terminated
  3. 3
    ろ過The resulting sodium chloride was filtered off
  4. 4
    濃縮the filtrate was concentrated
  5. 5
    その他dried in a vacuum
  6. 6
    workup.DISSOLUTIONThe residue was dissolved in dichloromethane
  7. 7
    ろ過the solution was again filtered with a membrane
  8. 8
    ろ過filter
  9. 9
    濃縮the filtrate was concentrated in a vacuum
  10. 10
    その他dried

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08366956B2uspto-grants-2013_02