Reaktion #343979

ord-07f892a4d3304c3596ab9f5fde776006

Lösungsmittel

Reaktionsbedingungen

Temperatur
140°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigewater collected as the reaction
  2. 2
    Waschenby washing three times with 50 ml saturated sodium bicarbonate solution
  3. 3
    SonstigeThe organic layer was collected
  4. 4
    Trocknendried over magnesium sulfate
  5. 5
    SonstigeExcess decyl alcohol was removed by high vacuum distillation

Vorschrift

A 50 ml one neck round bottom flask equipped with a Dean Stark trap, condenser and a nitrogen inlet/outlet was charged with 5.0 g (0.038 moles) DL-2-hydroxycaproic acid, 23.95 g (0.151 moles) decyl alcohol, and 0.019 g sulfuric acid. The reactants were heated to 140° C. for 8 hours and water collected as the reaction proceeded. The acid was neutralized by washing three times with 50 ml saturated sodium bicarbonate solution. Approximately 50 ml ether was needed to break the emulsion. The organic layer was collected and dried over magnesium sulfate. Excess decyl alcohol was removed by high vacuum distillation to yield 4.34 g (49% yield) of clear colorless liquid. According to GC the product is 95.74% pure.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05260051uspto-grants-1993_11