反应 #470366

ord-96ecff76950647ebafe1a913cd6feca8

反应方程式

[F-].[K+]
potassium fluoride
COC[N+]1(C)CCCC1.[O-][Cl+3]([O-])([O-])[O-]
N-methoxymethyl-N-methylpyrrolidinium perchlorate
COC[N+]1(C)CCCC1.[F-]
desired product
COC[N+]1(C)CCCC1.[F-]
N-Methoxymethyl-N-Methylpyrrolidinium Fluoride

溶剂

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
    workup.ADDITIONWith addition of 100 ml of methanol
  4. 4
    过滤the reaction mixture was filtered
  5. 5
    浓缩The filtrate was concentrated
  6. 6
    其他dried in a vacuum
  7. 7
    workup.DISSOLUTIONThe residue was then dissolved in dichloromethane
  8. 8
    过滤the solution was again filtered with a membrane
  9. 9
    过滤filter
  10. 10
    浓缩the filtrate was concentrated
  11. 11
    其他dried

实验过程

A 0.44 g quantity of potassium fluoride (product of Wako Pure Chemical Ind. Ltd.) was dissolved in 11 g of deionized water, and 1.74 g of N-methoxymethyl-N-methylpyrrolidinium perchlorate was added to the solution. The mixture was reacted at room temperature for 1.5 hours, whereby the reaction was terminated. With addition of 100 ml of methanol, the reaction mixture was filtered. The filtrate was concentrated and dried in a vacuum. The residue was then dissolved in dichloromethane, the solution was again filtered with a membrane filter, and the filtrate was concentrated and dried, giving 1.05 g of the desired product.

来源

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