Reaktion #658337

ord-7a6d1b98f67a4b15876d1ce5bb9dfedd

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeobtained by the 3rd step
  2. 2
    SonstigeSubsequently, an organic layer was separated
  3. 3
    Waschenthe thus obtained organic layer was rinsed with 20 g of water four times
  4. 4
    WaschenSubsequently, it was rinsed with 20 g of diisopropyl ether three times
  5. 5
    workup.DISTILLATIONa volatile component was distilled off

Vorschrift

A 50 mL reactor was charged with the triethylammonium 1,1-difluoro-2-(2-methyl-acryloyloxy)-ethane-1-sulfonate aqueous solution obtained by the 3rd step, and a solution of 3.18 g (8.9 millimoles) of triphenylsulfonium bromide and 20 g of chloroform, followed by 3 hours of stirring at room temperature. Subsequently, an organic layer was separated, and the thus obtained organic layer was rinsed with 20 g of water four times. Subsequently, it was rinsed with 20 g of diisopropyl ether three times and then a volatile component was distilled off, thereby obtaining 3.92 g of a target triphenylsulfonium 1,1-difluoro-2-(2-methyl-acryloyloxy)-ethane-1-sulfonate. It exhibited a purity of 97% at this time, and a yield of 87% taken over from the 3rd step.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09024058B2uspto-grants-2015_05