Reaktion #93593

ord-08896e7ec06642c78abc4d95b1516e9c

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONA mixture of 19.6 g
  2. 2
    Sonstigewhich was equipped with a Soxhlet extractor
  3. 3
    TemperaturThe mixture was heated
  4. 4
    Temperaturunder reflux
  5. 5
    SonstigeThe mixture obtained from the heating for a total of 26 hours
  6. 6
    workup.DISTILLATIONwas subjected to single distillation
  7. 7
    Sonstigeto give 24.24 g

Vorschrift

A mixture of 19.6 g. of methyl angelate, 22.2 g. of 3-methyl-2-butenyl alcohol, 100 ml. of toluene and 1.6 g. of dioctyltin laurate was placed in a glass flask which was equipped with a Soxhlet extractor filled with molecular sieve 4A on the top and a reflux cooler. The mixture was heated under reflux while returning the refluxed liquid through the molecular sieve 4A to the flask. The mixture obtained from the heating for a total of 26 hours was subjected to single distillation to give 24.24 g. of a distillate boiling at 102°-105° C. (25 mmHg).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04613680uspto-grants-1986_09