Reaktion #1569780

ord-57d7bc0cd97047cbbbbae1c320fe17e6

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONwere respectively added
  2. 2
    workup.ADDITIONmixed
  3. 3
    Temperaturheated
  4. 4
    Temperaturrefluxed
  5. 5
    Sonstigeto react for 15 hours
  6. 6
    Filtrationfiltered
  7. 7
    EinengenThe filtrate was concentrated
  8. 8
    Sonstigeto produce oily products
  9. 9
    workup.ADDITIONtreated by chromatography with neutral Al2O3
  10. 10
    Sonstigepurified
  11. 11
    Wascheneluted with dichloromethane

Vorschrift

1-(4-chlorobutyl)-1H-benzotriazole (7.55 g, 0.036 mol) was dissolved into 100 ml of acetonitrile, 3-cyano phenylpiperazine (5.6 g, 0.03 mol), diisopropylethylamine (15.5 g, 0.12 mol) and potassium iodide (5.0 g, 0.03 mol) were respectively added. The mixture was stirred and mixed, then heated and refluxed to react for 15 hours. The mixture was cooled down to ambient temperature and filtered. The filtrate was concentrated to produce oily products, and treated by chromatography with neutral Al2O3 and purified, eluted with dichloromethane to produce 7.6 g compound (I-41) with a yield of 70.5%. ESI-MS [M+H]+: m/z 360.2.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09415047B2uspto-grants-2016_08