Reaktion #2503540

ord-bfcf9ae7d5b047d3ac0c3a9ae7f6ea2f

Lösungsmittel

Reaktionsbedingungen

Temperatur
0°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeproduced
  2. 2
    Extraktionthe product was extracted with toluene (50 mL)
  3. 3
    TrocknenThe toluene layer was dried on anhydrous magnesium sulfate
  4. 4
    workup.DISTILLATIONthe solvent was distilled off under reduced pressure
  5. 5
    SonstigeThe resulting residue was purified by means of column chromatography (silica gel, eluting solvent: toluene)

Vorschrift

Acetic anhydride (5 mL) was slowly added to a mixture of 4-(2-(2-pentyloxyfluorene-7-yl)ethyl)phenol (5 g) produced according to the first to ninth steps in Example 1 and pyridine (100 mL) while maintaining 0° C., and the solution was stirred at the same temperature for 2 hours. The reaction mixture was poured into ice and water (200 mL), and the product was extracted with toluene (50 mL). The toluene layer was dried on anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The resulting residue was purified by means of column chromatography (silica gel, eluting solvent: toluene) to obtain 4-(2-(2-pentyloxyfluorene-7-yl)ethyl)phenyl acetate (5.1 g).

Quelle

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