Reacción #166209

ord-0fdb007c69104fa0a5cb5b6cc2588bbd

Disolventes

Condiciones de reacción

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

Tratamiento posterior

  1. 1
    OtroThe volatile solvent was removed in vacuo
  2. 2
    Temperaturawhilst applying cooling
  3. 3
    FiltraciónThe resultant precipitate was collected by filtration
  4. 4
    Lavadowashed with water

Procedimiento

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.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08841462B2uspto-grants-2014_09