Reaktion #41820

ord-f61cc33c144f484db6ec21ca0b119229

Lösungsmittel

Reaktionsbedingungen

Temperatur
75°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturto cool to room temperature for 15 h
  2. 2
    TemperaturThe reaction mixture was cooled further to 0° C.
  3. 3
    workup.STIRRINGwas then stirred for 2 h
  4. 4
    FiltrationThe resulting precipitate was collected by suction filtration
  5. 5
    Waschenwashed with cold EtOH (20 mL)
  6. 6
    SonstigeThe wet solid was dried in a vacuum oven at 40° C. for 6 h

Vorschrift

To a solution of (4-isopropyl-piperazin-1-yl)-(4-morpholin-4-ylmethyl -phenyl)-methanone (3.0 g, 9.05 mmol) in absolute EtOH (20 mL) was added, via an addition funnel, a solution of maleic acid (3.3 g, 19.8 mmol) in absolute EtOH (20 mL) over 10 min. The resulting suspension was stirred at room temperature for 15 min, at 75° C. for 30 min, and was then allowed to cool to room temperature for 15 h. The reaction mixture was cooled further to 0° C. and was then stirred for 2 h. The resulting precipitate was collected by suction filtration and washed with cold EtOH (20 mL). The wet solid was dried in a vacuum oven at 40° C. for 6 h to yield the title compound as crude material, as a white solid.

Quelle

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