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

HRID 560988노트

반응식

HRID 560988 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-a599556fa1394627a8e00bb15c5ac4df
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08063206B2

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