Maleic Acid → 4-Amino-N-[2-(4-benzoylpiperidino)ethyl]-N-(3-pyridyl)benzamide maleate

HRID 2527

Reaktionsgleichung

Reaktionsgleichung von HRID 2527
[NH2:1][C:2]1[CH:32]=[CH:31][C:5]([C:6]([N:8]([CH2:15][CH2:16][N:17]2[CH2:22][CH2:21][CH:20]([C:23](=[O:30])[C:24]3[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=3)[CH2:19][CH2:18]2)[C:9]2[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=2)=[O:7])=[CH:4][CH:3]=1.[C:33]([OH:40])(=[O:39])/[CH:34]=[CH:35]\[C:36]([OH:38])=[O:37]>C(O)C>[C:33]([OH:40])(=[O:39])/[CH:34]=[CH:35]\[C:36]([OH:38])=[O:37].[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:6]([N:8]([CH2:15][CH2:16][N:17]2[CH2:18][CH2:19][CH:20]([C:23](=[O:30])[C:24]3[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=3)[CH2:21][CH2:22]2)[C:9]2[CH:10]=[N:11][CH:12]=[CH:13][CH:14]=2)=[O:7])=[CH:31][CH:32]=1

Komponenten

4

Edukt 2

HCID 444266Maleic AcidHCID 98888325-HT2A antagonist 1

Produkt 1

HCID 676729174-Amino-N-[2-(4-benzoylpiperidino)ethyl]-N-(3-pyridyl)benzamide maleateAusbeute 65 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

4-Amino-N-[2-(4-benzoylpiperidino)ethyl]-N-(3-pyridyl)benzamide (3.00 g, 7.00 mmol) was dissolved in ethanol (10.0 ml) to which was subsequently added a ethanol solution (20.0 ml) of maleic acid (812.0 mg, 7.00 mmol) at room temperature, and then stirred. After the solvent was removed by evaporation, the thus precipitated crystals were collected by filtration and washed with ether, and then purified by recrystallization from ethanol-water mixed solution to obtain 2.476 g (65%) of the title compound in a colorless powder form.

Aufarbeitung

  1. customAfter the solvent was removed by evaporation
  2. filtrationthe thus precipitated crystals were collected by filtration
  3. washwashed with ether
  4. custompurified by recrystallization from ethanol-water mixed solution

Quellen und Nachweise

ORD-Eintrag
ord-5dbd58a197604caab9440bf88042ff6e
Quelldatensatz
uspto-grants-1998_03
Patentnummer
US05728835

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