Reaktion #215168

ord-19153b4326cc40869366b62e207e42f0

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturis heated
  2. 2
    Temperaturat reflux for one-half four
  3. 3
    workup.DISTILLATIONBy-product methanol is distilled off
  4. 4
    workup.ADDITIONadditional methyl formate (20 ml.) added
  5. 5
    TemperaturThe mixture is refluxed for a half hour
  6. 6
    Sonstigethe white solid residue recrystallized from ethyl acetate
  7. 7
    SonstigeYield=quantitative

Vorschrift

A mixture of N,N-dioctadecyl-1,3-propanediamine (4.88 g.), ethanol (15 ml.) and methyl formate (35 ml.) is heated at reflux for one-half four. By-product methanol is distilled off and additional methyl formate (20 ml.) added. The mixture is refluxed for a half hour and allowed to stand overnight. It is taken to dryness under reduced pressure and the white solid residue recrystallized from ethyl acetate. Yield=quantitative: m.p. 42°-46° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04258061uspto-grants-1981_03