Reaktion #2375062

ord-272499fe351447f69dfe67a1403361ec

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigePurification
  2. 2
    Wascheneluting with 4:1 hexane/acetone
  3. 3
    Sonstigeafforded an oil that
  4. 4
    Sonstigerecrystallized from EtOAc/MeOH

Vorschrift

Using procedure 47, 2-[(4-Chlorophenyl)methyl]-6-(dipropylamino)-6,7-dihydrocyclopent[f]isoindole-1,3(2H,5H)-dione (102, 0.59 g, 1.43 mmol) was reduced with Zinc dust (0.94 g, 14.3 mmol) in glacial HOAc (100 mL). Purification using silica gel, eluting with 4:1 hexane/acetone, afforded an oil that was converted to an HCl salt and recrystallized from EtOAc/MeOH to give 129 as a white solid (m.p. 233-234° C.).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06084130uspto-grants-2000_07