Reacción #70091

ord-00a9ac1db27b40b09212abd489d8cc84

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturathe mixture was heated
  2. 2
    Temperaturaunder reflux
  3. 3
    Otrofor 12 h
  4. 4
    OtroAfter that, toluene was removed under reduced pressure
  5. 5
    workup.DISSOLUTIONthe crude mixture was dissolved in dichloromethane (200 ml)
  6. 6
    Extracciónextracted with water (pH 5, 3×200 ml)
  7. 7
    SecadoThe combined organic layers were dried over sodium sulfate
  8. 8
    Otrothe volatiles were removed under reduced pressure

Procedimiento

2-propylpentanoic acid (10.0 g, 69.3 mmol) was mixed with propane-1-3-diol (42.1 g, 555.0 mmol) and methyl-sulfonic acid (5 drops) in toluene (200 ml) and the mixture was heated under reflux using a Dean Stark trap for 12 h. After that, toluene was removed under reduced pressure and the crude mixture was dissolved in dichloromethane (200 ml) and extracted with water (pH 5, 3×200 ml). The combined organic layers were dried over sodium sulfate and the volatiles were removed under reduced pressure giving a clear oil (14.0 g, 60.0 mmol, 99%).

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08535655B2uspto-grants-2013_09