Reaktion #1590392

ord-aaa65a21822d49259296ebf3080a7d51

Reaktionsbedingungen

Temperatur
140°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwas added
  2. 2
    Extraktionthe mixture was extracted
  3. 3
    TrocknenThe organic layer was dried over anhydrous sodium sulfate
  4. 4
    Einengenthe solvent was concentrated under reduced pressure

Vorschrift

Under an argon atmosphere, 3-chloro[1,4]benzodioxino[2,3-c]pyridazine (5.0 g), sodium iodide (6.79 g) and hydrogen iodide (55%) (57.98 g) were added and the mixture was stirred at 140° C. for 1 hr. The reaction mixture was diluted with ethyl acetate and aqueous sodium hydrogen carbonate solution was added, and the mixture was extracted. The organic layer was dried over anhydrous sodium sulfate, and the solvent was concentrated under reduced pressure to give 3-iodo[1,4]benzodioxino[2,3-c]pyridazine (1.95 g).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09212147B2uspto-grants-2015_12