Reaktion #75057

ord-f0616c2b746642858f6b65dc1ecff7f3

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture is then refluxed for 3 hours
  2. 2
    Temperaturafter cooling
  3. 3
    Einengenconcentrated to 166 of its original volume by rotary evaporation
  4. 4
    workup.ADDITIONThe residue is poured into ice-water
  5. 5
    ExtraktionAfter extraction with ether
  6. 6
    Waschenthe organic phase is washed three times with saturated sodium chloride solution
  7. 7
    Trocknendried over sodium sulphate
  8. 8
    Einengenconcentrated by rotary evaporation
  9. 9
    workup.DISTILLATIONDistillation of the residue

Vorschrift

A solution of 1.68 g of potassium hydroxide in 20 ml of water is added at room temperature to a solution of 6.24 g of 1-acetoxy-2-(4-phenoxyphenoxy)-cyclopentane in 50 ml of ethanol. The mixture is then refluxed for 3 hours and, after cooling, concentrated to 166 of its original volume by rotary evaporation. The residue is poured into ice-water. After extraction with ether, the organic phase is washed three times with saturated sodium chloride solution, dried over sodium sulphate and concentrated by rotary evaporation. Distillation of the residue yields 2-(4-phenoxyphenoxy)-cyclopentan-1-ol as a colourless oil with a boiling point of 181°-185° C./0.001 torr.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04175137uspto-grants-1979_11