Reacción #41954

ord-fc9b9235d9cf49359251140b795631d9

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

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

Procedimiento

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%.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07728152B2uspto-grants-2010_06