Reaktion #5842

ord-98066fc44b1d4119929f1efebf1ad116

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.STIRRINGfurther stirred at a room temperature overnight
  2. 2
    SonstigeAfter evaporating off the pyridine under a reduced pressure
  3. 3
    Extraktionthe mixture was extracted twice with 50 ml of chloroform/isopropanol (10:1)
  4. 4
    TrocknenThe extract was dried over magnesium sulfate
  5. 5
    Sonstigeevaporated under a reduced pressure
  6. 6
    Sonstigeto remove the solvent
  7. 7
    workup.ADDITIONTo the resulting residue was added 20 ml of benzene/chloroform (3:1)
  8. 8
    Temperaturthe mixture was slightly warmed
  9. 9
    Sonstigecollected

Vorschrift

3.06 g of 3,4-dimethoxyaniline was dissolved in 30 ml of pyridine, to the solution was added in small portions 5.28 g of 5-isoquinolinesulfonyl chloride.HCl with stirring under ice cooling, and the mixture was stirred for 30 minutes, and further stirred at a room temperature overnight. After evaporating off the pyridine under a reduced pressure and additing 20 ml of water, the mixture was extracted twice with 50 ml of chloroform/isopropanol (10:1). The extract was dried over magnesium sulfate and evaporated under a reduced pressure to remove the solvent. To the resulting residue was added 20 ml of benzene/chloroform (3:1), and the mixture was slightly warmed and collected to obtain 5.64 g of the title compound as colorless crystals.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05245034uspto-grants-1993_09