Réaction #70095

ord-bfee8a1339084b148a77c82b91b7385d

Solvants

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températurethe mixture was heated
  2. 2
    Températureunder reflux
  3. 3
    Autrefor 12 h
  4. 4
    AutreAfter that, toluene was removed under reduced pressure
  5. 5
    workup.DISSOLUTIONthe crude mixture was dissolved in chloroform (200 ml)
  6. 6
    Extractionextracted with water (pH 5, 3×200 ml)
  7. 7
    SéchageThe combined organic layers were dried over sodium sulfate
  8. 8
    Autrethe volatiles were removed under reduced pressure

Mode opératoire

2-propylpentanoic acid (40.16 g, 278.5 mmol) was mixed with butane-1-4-diol (114.65 g, 1272.2 mmol) and methyl-sulfonic acid (5 drops) in toluene (3500 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 chloroform (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 (99%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US08535655B2uspto-grants-2013_09