Reaktion #2983

ord-ff41cf49840a4862bb629df3394008db

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONIt is poured into ice
  2. 2
    ExtraktionIt is extracted with 3 volumes of ether
  3. 3
    WaschenThe organic phases are washed 3 times with 10% potassium carbonate solution
  4. 4
    workup.ADDITIONby adding concentrated hydrochloric acid until the pH is 3-4
  5. 5
    SonstigeThe precipitate obtained
  6. 6
    Sonstigerecrystallized

Vorschrift

In a 100-cm3 flask, 2.5 g of 4-oxo-4-(4-ethylphenyl)butyric acid are dissolved with magnetic stirring in 19 cm3 of trifluoroacetic acid. 3.2 g of triethylsilane are added dropwise. The reaction mixture is stirred for 86 hours at room temperature. It is poured into ice. It is extracted with 3 volumes of ether. The organic phases are washed 3 times with 10% potassium carbonate solution. The aqueous phases are combined and then acidified by adding concentrated hydrochloric acid until the pH is 3-4. The precipitate obtained is drained and then recrystallized.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05731352uspto-grants-1998_03