Reacción #334982

ord-2515ebd924874b8ba0035998e527f816

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Extracciónextraction
  2. 2
    workup.DISTILLATIONthe extracted layer was distilled
  3. 3
    Otroto remove the solvent
  4. 4
    workup.ADDITIONThe residue was added to a solution of sodium hydroxide (3 g)
  5. 5
    Temperaturawater (10 ml) and ethanol(50 ml) and the solution was refluxed for about one day
  6. 6
    workup.DISTILLATIONdistilled
  7. 7
    Otroto remove the solvent
  8. 8
    Concentraciónconcentrated
  9. 9
    OtroSolid collected
  10. 10
    Otrowas recrystallized from water/ethanol

Procedimiento

A solution of dodecylbromide (8.2 g, 4-hydroxybenzoic acid (5 g) and potassium carbonate (5 g) in dimethylformamide (100 ml) was stirred at 130° C. for two hours. The solution was poured in water and neutralized with dilute aqueous hydrochloric acid solution. Diethyl ether was added in order to effect extraction and the extracted layer was distilled to remove the solvent. The residue was added to a solution of sodium hydroxide (3 g). water (10 ml) and ethanol(50 ml) and the solution was refluxed for about one day. The solution was neutralized with dilute aqueous hydrochloric acid solution and distilled to remove the solvent and concentrated. Solid collected was recrystallized from water/ethanol to obtain the titled compound (4.9 g).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US05207947uspto-grants-1993_05