Reacción #171752

ord-7b9c5fd6baea4459ba7215a91149f033

Disolventes

Condiciones de reacción

Temperatura
90°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroThe whole was sealed
  2. 2
    Temperaturacooled to room temperature
  3. 3
    Concentraciónconcentrated
  4. 4
    workup.ADDITIONThe residue was diluted with water
  5. 5
    Extracciónextracted with ethyl acetate
  6. 6
    OtroThe combined organics were purified by reverse phase HPLC

Procedimiento

To a solution of crude 2-(2-chlorophenyl)-1-(4,5-dihydrobenzo[b]thieno[2,3-d]oxepin-2-yl)-3-(dimethylamino)prop-2-en-1-one (ca. 0.22 mmol) in ethanol (2 mL) was added potassium carbonate (87 mg, 0.63 mmol) and then guanidine hydrochloride (40 mg, 0.42 mmol). The whole was sealed and heated at 90° C. for 8 h, cooled to room temperature and concentrated. The residue was diluted with water and extracted with ethyl acetate. The combined organics were purified by reverse phase HPLC to give 282. MS (ESI) 406.2

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08846762B2uspto-grants-2014_09