Reaktion #92782

ord-d9a54e4d69f34c5d96fd25a0d6324924

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwas heated
  2. 2
    Temperaturto reflux for 6 hours
  3. 3
    SonstigeThe water liberated was collected in a Dean Stark trap
  4. 4
    TemperaturThe mixture was cooled
  5. 5
    Waschenwashed with saturated sodium bicarbonate (300 mL) and brine (100 mL)
  6. 6
    Trocknendried over magnesium sulfate
  7. 7
    SonstigeThe solvent was removed under vacuum
  8. 8
    Sonstigeto give a yellow oil that
  9. 9
    Sonstigewas used without further purification (426.39 g)

Vorschrift

A mixture of succinic acid (Alfa-Aesar, 149.00 g, 1.26 mol), 2-octanol (Alfa-Aesar, 350.00 g, 2.69 mol), toluene (625 mL), and methanesulfonic acid (Alfa-Aesar, 2.00 g, 21 mmol) was heated to reflux for 6 hours. The water liberated was collected in a Dean Stark trap. The mixture was cooled, washed with saturated sodium bicarbonate (300 mL) and brine (100 mL), and dried over magnesium sulfate. The solvent was removed under vacuum to give a yellow oil that was used without further purification (426.39 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09447309B2uspto-grants-2016_09