Reaktion #89618

ord-59cafe26ff9e483eae52495a7a1c2ddb

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was heated
  2. 2
    Temperaturto reflux for 6 hours
  3. 3
    Sonstigequenched with aqueous sodium bicarbonate (1 L)
  4. 4
    WaschenThe reaction mixture was then washed with brine (0.5 L)
  5. 5
    Trocknendried over sodium sulfate (50 g)
  6. 6
    SonstigeThe solvent was removed
  7. 7
    workup.DISTILLATIONthe reaction mixture was distilled

Vorschrift

2-Heptanol (200 g, 1.72 mol) and cyclopropanecarboxylic acid (163 g, 1.90 mol) were added into toluene (500 mL), followed by p-toluenesulfonic acid (3.2 g, 0.0172 mol). The reaction mixture was heated to reflux for 6 hours, cooled to room temperature, and quenched with aqueous sodium bicarbonate (1 L). The reaction mixture was then washed with brine (0.5 L) and dried over sodium sulfate (50 g). The solvent was removed and the reaction mixture was distilled to provide the product cyclopropanecarboxylic acid 1-methyl-hexyl ester (253 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09441185B2uspto-grants-2016_09