Reaktion #533389

ord-960885f55734451fb729924cbf137bb5

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigethe reaction at 70° C. for 5.5 hours under a hydrogen pressure of 4 MPa
  2. 2
    SonstigeThe thus obtained reaction solution
  3. 3
    Sonstigewas subjected to evaporation of the solvent
  4. 4
    workup.DISTILLATIONdistilled under a reduced pressure (121° C./170 Pa)

Vorschrift

144.2 g (0.60 mol) of 1-menthyl acetoacetate, 98.8 mg (12.0 μmol) of a catalyst [{RuCl((R)-SEGPHOS)}2(μ-Cl)3][NH2Me2] and 75 ml of methanol were put into a 500 ml capacity autoclave and allowed to undergo the reaction at 70° C. for 5.5 hours under a hydrogen pressure of 4 MPa. The thus obtained reaction solution was subjected to evaporation of the solvent and then distilled under a reduced pressure (121° C./170 Pa) to obtain 143.1 g (yield 98.4%) of the (3R)-1-menthyl 3-hydroxybutyrate of interest as a colorless oily substance.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08476472B2uspto-grants-2013_07