Reaktion #806454

ord-c3566224417b4e6a9e73d32bf62313da

Lösungsmittel

Reaktionsbedingungen

Temperatur
40°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe resulting suspension was filtered with suction through silica gel
  2. 2
    Einengenafter which the filtrate was concentrated under reduced pressure
  3. 3
    Sonstigethe residue was purified by means of HPLC (Merk-Hibar-Lichrospher 100-RP-18, water (0.1% trifluoroacetic acid)/acetonitrile (0.1% trifluoroacetic acid)=80/20→10/90)
  4. 4
    SonstigeThe following was obtained

Vorschrift

2.1 g of potassium permanganate in 36 ml of water were added to a solution of 600 mg of 5-phenyl-3-methyl-1H-pyrazolo[4,3-c]isoquinoline in 36 ml of pyridine. The mixture was stirred at 40° C. for 12 h. The resulting suspension was filtered with suction through silica gel, after which the filtrate was concentrated under reduced pressure and the residue was purified by means of HPLC (Merk-Hibar-Lichrospher 100-RP-18, water (0.1% trifluoroacetic acid)/acetonitrile (0.1% trifluoroacetic acid)=80/20→10/90). The following was obtained: 60.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07132428B2uspto-grants-2006_11