反応 #470366

ord-96ecff76950647ebafe1a913cd6feca8

反応方程式

[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

溶媒

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

実験手順

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.

出典

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