Reaktion #968010

ord-ac7226b3b76142e385f36bc32fd46050

Lösungsmittel

Reaktionsbedingungen

Temperatur
55°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe solvent was removed under reduced pressure
  2. 2
    workup.ADDITIONthe residue was diluted with dichloromethane
  3. 3
    Waschenwashed twice with aqueous sodium hydrogencarbonate saturated solution
  4. 4
    TrocknenThe combined organic layer were dried over sodium sulphate
  5. 5
    Einengenconcentrated under reduced pressure

Vorschrift

To a solution of 590 mg (1.54 mmol) of 7-fluoro-3-phenyl-4-[2-(tetrahydro-2H-pyran-2-yloxy)ethoxy]isoquinolin-1(2H)-one in methanol (12 mL), 88 mg of p-toluenesulphonic acid (0.46 mmol) were added and the resulting mixture was heated at 55° C. for 2 hours. The solvent was removed under reduced pressure and the residue was diluted with dichloromethane and washed twice with aqueous sodium hydrogencarbonate saturated solution. The combined organic layer were dried over sodium sulphate and concentrated under reduced pressure to afford 438 mg of the title compound (95%).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08993594B2uspto-grants-2015_03