반응 #166209

ord-0fdb007c69104fa0a5cb5b6cc2588bbd

용매

반응 조건

온도
90°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The volatile solvent was removed in vacuo
  2. 2
    온도whilst applying cooling
  3. 3
    여과The resultant precipitate was collected by filtration
  4. 4
    세척washed with water

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08841462B2uspto-grants-2014_09