Reaktion #68844

ord-76001af253f34f63a8e9af4acd8ded6a

Lösungsmittel

Reaktionsbedingungen

Temperatur
80°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONare added
  2. 2
    Extraktionextracted with EtOAc
  3. 3
    Trocknendried with Na2SO4
  4. 4
    Sonstigethe solvent is removed in vacuo
  5. 5
    SonstigeThe resulting crude product is triturated with TBME

Vorschrift

20 mL ACN are added to 0.50 g (1.11 mmol) 3-(4-chlorophenyl)-6-chloropyridazine and 3.33 g (22.2 mmol) NaI before 189 μl fuming conc. HCl are added and the mixture is stirred at 80° C. for 4 h. The mixture is alkalised with aq. ammonia solution (32%) diluted with water and extracted with EtOAc. The org. phases are combined, dried with Na2SO4 and the solvent is removed in vacuo. The resulting crude product is triturated with TBME.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08530460B2uspto-grants-2013_09