Reaktion #166222

ord-edd1d763f8bd491ab56369709c4a27f4

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeat room temperature
  2. 2
    SonstigeThe organic solvent was removed in vacuo
  3. 3
    workup.ADDITIONthe mixture diluted with water (50 mL)
  4. 4
    FiltrationThe resulting solid was collected by filtration
  5. 5
    Waschenwashed with water
  6. 6
    Sonstigedried under vacuum

Vorschrift

To a stirred solution of 6-fluoro-2-(2-fluoro-4-iodo-phenylamino)-3-nitro-benzaldehyde (864 mg, 2.14 mmol) in DME (15 ml) was slowly added hydrazine hydrate (10 mL) at room temperature and the reaction mixture stirred for 18 hours. The organic solvent was removed in vacuo and the mixture diluted with water (50 mL). The resulting solid was collected by filtration, washed with water and dried under vacuum to yield the title compound (839 mg, 98%). LCMS (Method B): RT=3.61 min, [M+H]+=399.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08841462B2uspto-grants-2014_09