Maleic Acid → (4-Isopropyl-piperazin-1-yl)-(4-piperidin-1-ylmethyl-phenyl)-methanone, bis-maleate salt

HRID 560988Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 560988
[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]([C:12]2[CH:17]=[CH:16][C:15]([CH2:18][N:19]3[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]3)=[CH:14][CH:13]=2)=[O:11])[CH2:6][CH2:5]1)([CH3:3])[CH3:2].[C:25]([OH:32])(=[O:31])/[CH:26]=[CH:27]\[C:28]([OH:30])=[O:29]>CCO.CCOCC>[C:25]([OH:32])(=[O:31])/[CH:26]=[CH:27]\[C:28]([OH:30])=[O:29].[C:25]([OH:32])(=[O:31])/[CH:26]=[CH:27]\[C:28]([OH:30])=[O:29].[CH:1]([N:4]1[CH2:9][CH2:8][N:7]([C:10]([C:12]2[CH:17]=[CH:16][C:15]([CH2:18][N:19]3[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]3)=[CH:14][CH:13]=2)=[O:11])[CH2:6][CH2:5]1)([CH3:3])[CH3:2]

Komponenten

5

Edukt 2

HCID 444266Maleic AcidHCID 10359235(1-Isopropylpiperidin-4-yl)(4-(piperidin-1-ylmethyl)phenyl)methanone

Produkt 1

HCID 131728158(4-Isopropyl-piperazin-1-yl)-(4-piperidin-1-ylmethyl-phenyl)-methanone, bis-maleate salt

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittel2×HCID 3283Diethyl EtherLösungsmittel

Versuchsvorschrift

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.

Aufarbeitung

  1. temperaturecooled to 0° C.
  2. stirringstirred for 2 h
  3. filtrationThe precipitate was collected by suction filtration
  4. washwashed with cold EtOH/Et2O (4:1, 3×100 mL)
  5. customThe solids were dried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-a599556fa1394627a8e00bb15c5ac4df
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08063206B2

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