Reaktion #348724

ord-12a704a9055f43ae94b8f6baaf13e640

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux for one hour
  2. 2
    EinengenThe cooled solution is concentrated
  3. 3
    workup.ADDITIONdiluted with water
  4. 4
    Extraktionthe neutral components are extracted with ether
  5. 5
    Extraktionextracted with ether
  6. 6
    Extraktionthe ether extract
  7. 7
    Waschenis washed with water
  8. 8
    Trocknendried over sodium sulphate
  9. 9
    Einengenconcentrated by evaporation
  10. 10
    SonstigeThe resulting 2-ethyl-6-chloro-2-methyl-5-indanacetic acid is recrystallized from hexane

Vorschrift

A solution of 20 g of potassium hydroxide in 40 cc of water is added to a solution of 11.5 g of 2-ethyl-6-chloro-2-methyl-5-indanacetic acid methyl ester in 250 cc of methanol, and the solution is boiled at reflux for one hour. The cooled solution is concentrated, diluted with water and the neutral components are extracted with ether. The aqueous phase is acidified with hydrochloric acid, extracted with ether, the ether extract is washed with water, dried over sodium sulphate and concentrated by evaporation. The resulting 2-ethyl-6-chloro-2-methyl-5-indanacetic acid is recrystallized from hexane and has a M.P. of 87°-89°.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04166131uspto-grants-1979_08