Reaction #41955

ord-b38bb05c9a654ded9acc8930760c2a49

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    Temperatureby refluxing
  2. 2
    FiltrationAfter filtration
  3. 3
    Otherthe organic layer was separated
  4. 4
    Concentrationwas subjected to vacuum concentration
  5. 5
    workup.DISTILLATIONto Kugelrohr distillation at 110-120° C.

Procedure

Chloroacetaldehyde diethyl acetal (2.00 g), potassium benzoate (1.91 g), potassium iodide (0.41 g) and DMF (20 mL) were placed in a three-neck flask, followed by refluxing. Twenty hours later, the reaction mixture was cooled to room temperature, and water (30 mL) and ethyl acetate (80 mL) were added thereto, followed by stirring. After filtration, the organic layer was separated, was subjected to vacuum concentration and then to Kugelrohr distillation at 110-120° C. and at 1 mmHg and thereby yielded the target compound (2.41 g) in a yield of 77%.

Source

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