Reaktion #49746

ord-d09c4caf94244880bad4145de2e29eb2

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwhile heating
  2. 2
    Temperaturunder refluxing
  3. 3
    SonstigeAfter completion of the reaction
  4. 4
    workup.DISTILLATIONthe solvent was distilled off
  5. 5
    Sonstigeto obtain a crude product (37 g)
  6. 6
    WaschenThe product was washed with a mixed solvent of benzene/hexane

Vorschrift

2-Fluoro-4-chloro-5-cyclopentyloxyphenylhydrazine (24.5 g, 0.10 mol), 2-ethoxycarbonylcyclohexanone (17.0 g, 0.10 mol) were dissolved in acetic acid (200 ml), and stirred for 2 hours while heating under refluxing. After completion of the reaction, the solvent was distilled off to obtain a crude product (37 g). The product was washed with a mixed solvent of benzene/hexane to obtain 2N-(2-fluoro-4-chloro-5-cyclopentyloxyphenyl)-1,2,4,5,6,7-hexahydro-3H-indazol-3-one as a white solid (25.3 g, 72.3% yield)

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05424277uspto-grants-1995_06