Reaktion #362822

ord-f976a1c80cee43148409f29d61662ecf

Reaktionsbedingungen

Temperatur
160°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigein a transesterification reaction
  2. 2
    Sonstigepurged with nitrogen
  3. 3
    Sonstigeinserted with overhead stirrer
  4. 4
    SonstigeAt this temperature over 2 ml of methanol was collected
  5. 5
    TemperaturThe contents were heated to 200° C. with a nitrogen sweep
  6. 6
    Sonstigeto remove any volatile components
  7. 7
    TemperaturAfter approximately 15 minutes at 200° C. the contents were cooled
  8. 8
    TemperaturUpon cooling the product
  9. 9
    Sonstigecrystallized

Vorschrift

Behenyl Lactate was prepared by reacting methyl lactate (Aldrich Chemical Company, Inc. of Milwaukee, Wis.) with Lanette 22 (behenyl alcohol, 90%, Henkel Corp. of Ambler, Pa.) in a transesterification reaction according to the following method: 0.2 g sodium hydride (60% in mineral oil) was added to 32.6 grams Lanette 22 at 70° C. in a 3-neck 250ml glass flask purged with nitrogen and inserted with overhead stirrer, Dean Stark trap, thermometer, and condenser. To this was slowly added 9.4 g of methyl lactate and the contents were slowly heated to 160° C. and held at that temperature for one hour. At this temperature over 2 ml of methanol was collected. The contents were heated to 200° C. with a nitrogen sweep to remove any volatile components. After approximately 15 minutes at 200° C. the contents were cooled. Upon cooling the product crystallized and had a melting point of approximately 57° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06352701B1uspto-grants-2002_03