Reaktion #1686619

ord-be826166c97640f9a17881b400d0fbc0

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe catalyst was then removed by filtration
  2. 2
    Sonstigethe filtrate evaporated to dryness
  3. 3
    workup.ADDITIONAddition of dichloromethane (100 ml) to the residue and trituration
  4. 4
    Sonstigegave a solid which
  5. 5
    Sonstigewas recrystallised from methanol

Vorschrift

A mixture of 1-diphenylmethyl-3-morpholinoazetidine (Preparation 1(c)) (18.6 g, 60.4 mmol), palladium hydroxide (2 g), ethanol (200 ml) and 1N aqueous HCl (52 ml) was stirred under an atmosphere of hydrogen at 345 kPa (50p.s.i.) for 3 days. The catalyst was then removed by filtration and the filtrate evaporated to dryness. Addition of dichloromethane (100 ml) to the residue and trituration gave a solid which was recrystallised from methanol to give the title compound (10.2 g) as a crystalline solid. LRMS m/z=179 (m+1)+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05741790uspto-grants-1998_04