Reaktion #73098

ord-9b95dfc3a79647eb97fd830507e6bf5e

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was refluxed for 18 h
  2. 2
    Extraktionextracted with DCM
  3. 3
    EinengenThe organic layer was concentrated
  4. 4
    Sonstigepurified by silica column chromatography

Vorschrift

To a stirred solution of isoquinoline 2-oxide (2-Im-9, 5.8 g) in 140 mL of acetonitrile, diethyl phosphoro-cyanidate (1.5 eq) was added under argon followed by slow addition of TEA (3.0 eq). The mixture was refluxed for 18 h and then extracted with DCM. The organic layer was concentrated and purified by silica column chromatography to give isoquinoline-1-carbonitrile (3-Im-9).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08541418B2uspto-grants-2013_09