Reaktion #480685

ord-be2b5d2ed29c42d2b0b0e5fbadd52c87

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONto the solution was added a solution
  2. 2
    ExtraktionThe aqueous solution was extracted twice with each 200 ml of chloroform
  3. 3
    Waschenthe organic phase was washed with water
  4. 4
    Einengenconcentrated
  5. 5
    Sonstigeto obtain a crude product
  6. 6
    Temperaturcooled
  7. 7
    FiltrationThe solid product was collected by filtration

Vorschrift

In a mixed solvent of 200 ml of water and 200 ml of methanol was dissolved 60 g of potassium perfluorobutanesulfonate, and to the solution was added a solution containing 49,5 g of phenacylthiophenium bromide dissolved in 300 ml of water. The aqueous solution was extracted twice with each 200 ml of chloroform, and the organic phase was washed with water and concentrated to obtain a crude product. To the crude product was added 300 ml of distilled water, the mixture was heated at 100° C. for 30 minutes and cooled to deposit a solid product. The solid product was collected by filtration and subjected to reslurry with diisopropyl ether to obtain 77 g of phenacylthiophenium perfluorobutanesulfonate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06808862B2uspto-grants-2004_10