Reaktion #41820
ord-f61cc33c144f484db6ec21ca0b119229
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Temperatur
75°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Temperaturto cool to room temperature for 15 h
- 2TemperaturThe reaction mixture was cooled further to 0° C.
- 3workup.STIRRINGwas then stirred for 2 h
- 4FiltrationThe resulting precipitate was collected by suction filtration
- 5Waschenwashed with cold EtOH (20 mL)
- 6SonstigeThe 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.