Réaction #2267057

ord-806f0db4e285436185823604d705889d

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Extractionthe solution was extracted with dichloromethane
  2. 2
    LavageThen the organic phase was washed with a 5% aqueous solution of tetramethylammonium hydroxide and water
  3. 3
    Concentrationconcentrated

Mode opératoire

60 g of t-amylbenzene, 39.5 g of potassium iodate, 81 g of acetic anhydride and 170 ml of dichloromethane were mixed together. Then 66.8 g of conc. sulfuric acid was slowly added dropwise thereinto under ice-cooling. After stirring under ice-cooling for 2 hours, the mixture was stirred at room temperature for additional 10 hours. 500 ml of water was added to the liquid reaction mixture under ice-cooling and the mixture was extracted with dichloromethane. The organic phase was washed with sodium hydrogencarbonate and water and then concentrated to give (4-t-amylphenyl)iodonium sulfate. This sulfate was added to a solution of tetramethylammonium pentafluorobenzenesulfonate in excess. After adding 500 ml of water, the solution was extracted with dichloromethane. Then the organic phase was washed with a 5% aqueous solution of tetramethylammonium hydroxide and water and then concentrated to give di(4-t-amylphenyl)iodonium pentafluorobenzenesulfonate (III-1).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US06887645B2uspto-grants-2005_05