Reacción #219180

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Disolventes

Condiciones de reacción

Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    Temperaturais refluxed for 20 hours
  2. 2
    OtroPartitioning of the reaction mixture between ethyl acetate and water, separation of the organic phase
  3. 3
    Otroby drying
  4. 4
    Otroevaporation of the solvent
  5. 5
    Otrogives the crude product
  6. 6
    OtroPurification by chromatography on silicagel

Procedimiento

A mixture of 4-[1-(4-bromophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine (0.083 g, 0.21 mmol, prepared according to Example 1), sodium bicarbonate (0.021 g, 0.25 mmol) and hydroxylamine hydrochloride (0.014 g, 0.21 mmol) in ethanol (5 ml) is refluxed for 20 hours. Partitioning of the reaction mixture between ethyl acetate and water, separation of the organic phase followed by drying and evaporation of the solvent gives the crude product. Purification by chromatography on silicagel yields the title compound as an E/Z-mixture, m.p. 198-201° C.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US07385061B2uspto-grants-2008_06