Reaktion #41830

ord-b22e260c0052493a81278911e289ad16

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled to 0° C.
  2. 2
    workup.STIRRINGstirred for 2 h
  3. 3
    FiltrationThe precipitate was collected by suction filtration
  4. 4
    Waschenwashed with cold EtOH/Et2O (4:1, 3×100 mL)
  5. 5
    SonstigeThe solids were dried under vacuum

Vorschrift

To a mechanically agitated solution of (4-isopropyl-piperazin-1-yl)-(4-piperidin-1-ylmethyl-phenyl)-methanone (40.0 g, 122 mmol) in absolute EtOH (800 mL) was added, via an addition funnel, a solution of maleic acid (28.2 g, 243 mmol) in absolute EtOH (200 mL) over 30 min. The resulting suspension was stirred at room temperature for 16 h, then diluted with Et2O (200 mL), cooled to 0° C., and stirred for 2 h. The precipitate was collected by suction filtration, washed with cold EtOH/Et2O (4:1, 3×100 mL). The solids were dried under vacuum to yield crude title compound as a white solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07728129B2uspto-grants-2010_06