Reacción #66360

ord-3e55703534c3446d9a70a19b91ef85a3

Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    workup.ADDITIONpoured
  2. 2
    FiltraciónThe yellow precipitate was filtered
  3. 3
    Lavadowashed with water
  4. 4
    Otrodried at 60° C. under reduced pressure for 1 hour

Procedimiento

To a solution of 1-(3-methoxy-phenyl)-2-pyridin-4-yl-ethanone (1 g, 4.40 mmol) in dry DMSO (22 mL) under nitrogen atmosphere solid potassium carbonate (1.8 g, 13.20 mmol, 3 eq) was added at room temperature, followed by carbon disulfide (0.796 mL, 13.20 mmol, 3 eq) and dibromomethane (0.926 mL, 13.20 mmol, 3 eq). The reaction mixture was stirred at room temperature for 3 hour and then poured into stirred iced water (150 mL). The yellow precipitate was filtered, washed with water and dried at 60° C. under reduced pressure for 1 hour to give 1.18 g (83%) of 2-[1,3]dithietan-2-ylidene-1-(3-methoxy-phenyl)-2-pyridin-4-yl-ethanone.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08524707B2uspto-grants-2013_09