Reaktion #41954

ord-fc9b9235d9cf49359251140b795631d9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturby refluxing
  2. 2
    FiltrationAfter filtration
  3. 3
    Extraktionthe filtrate was extracted with ethyl acetate (500 mL)
  4. 4
    EinengenThe organic layer was subjected to vacuum concentration
  5. 5
    workup.DISTILLATIONto vacuum distillation at 132-135° C.

Vorschrift

Chloroacetaldehyde dimethyl acetal (50.0 g), potassium benzoate (70.7 g), potassium iodide (6.66 g) and DMF (N,N-dimethylformamide) (250 mL) were placed in a three-neck flask, followed by refluxing. Twenty hours later, the reaction mixture was cooled to room temperature, and water (250 mL) and ethyl acetate (250 mL) were added thereto, followed by stirring. After filtration, the filtrate was extracted with ethyl acetate (500 mL). The organic layer was subjected to vacuum concentration and then to vacuum distillation at 132-135° C. and at 5 mmHg and thereby yielded the target compound (61.0 g) in a yield of 72%.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07728152B2uspto-grants-2010_06