Reaktion #168160

ord-e4d8077039814a3bafe8553d897353ca

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturat reflux with a Dean-Stark trap
  2. 2
    Sonstigeto remove water
  3. 3
    WaschenThe reaction mixture was washed with a small amount of water and brine
  4. 4
    Trocknendried over anhydrous Na2SO4
  5. 5
    Einengenconcentrated in vacuum

Vorschrift

To a solution of methyl 4-methyl-3-oxopentanoate (72 g, 0.5 mol) and ethylene glycol (56 g, 1 mol) in toluene (500 mL) was added 4-methylbenzenesulfonic acid (1.9 g, 0.01 mol). The mixture was stirred at reflux with a Dean-Stark trap to remove water. The reaction mixture was washed with a small amount of water and brine, dried over anhydrous Na2SO4, and concentrated in vacuum to give the crude (2-isopropyl-[1,3]dioxolan-2-yl)-acetic acid methyl ester (67 g 71% yield), which was used for the next step without further purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846668B2uspto-grants-2014_09