Reaktion #58726

ord-b2293f481fac4e9ebe40fbfcb33a65e9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Filtrationis filtered
  2. 2
    Sonstigetransferred to a round bottom flask
  3. 3
    TemperaturThe reaction mixture is refluxed overnight with a Dean-Stark trap
  4. 4
    Waschenwashed with sat. aq NaHCO3, brine
  5. 5
    Trocknendried (Na2SO4)
  6. 6
    SonstigeProduct 33 is not purified further

Vorschrift

The solution of product 32 in toluene, from the previous reaction, is filtered, transferred to a round bottom flask, and ethylene glycol (2.4 eq) is added, followed by p-toulenesulfonic acid (0.5 eq). The reaction mixture is refluxed overnight with a Dean-Stark trap, then cooled down to room temperature, washed with sat. aq NaHCO3, brine, and dried (Na2SO4). Product 33 is not purified further but used as is in the following step.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07423148B2uspto-grants-2008_09