反应 #470365

ord-067845310e5f4c2590528862f9eebda8

反应方程式

[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

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

实验过程

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.

来源

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