Reaktion #2503541

ord-0dc93ad15c8f4f4c83a47befb3e73ba1

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwhile refluxing
  2. 2
    Temperaturby heating
  3. 3
    Extraktionthe product was extracted with chloroform
  4. 4
    Trocknento dry the chloroform layer on anhydrous magnesium sulfate
  5. 5
    SonstigeA residue obtained
  6. 6
    workup.DISTILLATIONby distilling the solvent off from this organic layer
  7. 7
    Sonstigewas purified by means of column chromatography (silica gel, eluting solvent: toluene)

Vorschrift

Oxygen was blown into a solution comprising 4-(2-(2-pentyloxyfluorene-7-yl)ethyl)phenyl acetate (4.2 g), powdery potassium hydroxide (1.0 g) and 2-butanone (80 mL) for one hour while refluxing by heating, and the solution was further stirred at a room temperature for one hour. A hydrochloric acid aqueous solution was added thereto, and then the product was extracted with chloroform to dry the chloroform layer on anhydrous magnesium sulfate. A residue obtained by distilling the solvent off from this organic layer was purified by means of column chromatography (silica gel, eluting solvent: toluene) to obtain 4-(2-(2-pentyloxyfluorenone-7-yl)ethyl)phenyl acetate (2.3 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06824709B2uspto-grants-2004_11