Reaktion #166209

ord-0fdb007c69104fa0a5cb5b6cc2588bbd

Lösungsmittel

Reaktionsbedingungen

Temperatur
90°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe volatile solvent was removed in vacuo
  2. 2
    Temperaturwhilst applying cooling
  3. 3
    FiltrationThe resultant precipitate was collected by filtration
  4. 4
    Waschenwashed with water

Vorschrift

To a suspension of 4-fluoro-2-(2-fluoro-4-methylsulfanyl-phenylamino)-3-formyl-benzoic acid (105 mg, 0.32 mmol) in DME (5 mL) was added hydrazine hydrate (5 mL) and the reaction mixture heated at 90° C. for 18 hours. The volatile solvent was removed in vacuo and the residue acidified with concentrated HCl whilst applying cooling. The resultant precipitate was collected by filtration and washed with water to give the title compound as a tan solid (85 mg, 82%). LCMS (Method B) RT 3.12 [M+H]+ 318.

Quelle

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