Potassium Carbonate → 3-Methyl-2-[4-[4-(4-phenylpiperazinylmethyl)-benzoyl]benzylthio]-4H-pyrido[1,2-a]pyrimidin-4-one

HRID 1291391Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1291391
[SH:1][C:2]1[N:3]=[C:4]2[CH:13]=[CH:12][CH:11]=[CH:10][N:5]2[C:6](=[O:9])[C:7]=1[CH3:8].Br[CH2:15][C:16]1[CH:31]=[CH:30][C:19]([C:20]([C:22]2[CH:27]=[CH:26][C:25]([CH2:28]Br)=[CH:24][CH:23]=2)=[O:21])=[CH:18][CH:17]=1.Cl.[C:33]1([N:39]2[CH2:44][CH2:43][NH:42][CH2:41][CH2:40]2)[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:8][C:7]1[C:6](=[O:9])[N:5]2[CH:10]=[CH:11][CH:12]=[CH:13][C:4]2=[N:3][C:2]=1[S:1][CH2:15][C:16]1[CH:31]=[CH:30][C:19]([C:20](=[O:21])[C:22]2[CH:27]=[CH:26][C:25]([CH2:28][N:42]3[CH2:43][CH2:44][N:39]([C:33]4[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=4)[CH2:40][CH2:41]3)=[CH:24][CH:23]=2)=[CH:18][CH:17]=1

Komponenten

6

Edukt 4

HCID 11430Potassium CarbonateHCID 751641-Phenylpiperazinium chlorideHCID 23039244,4'-Bis(bromomethyl)benzophenoneHCID 189188982-mercapto-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

Produkt 1

HCID 189188383-Methyl-2-[4-[4-(4-phenylpiperazinylmethyl)-benzoyl]benzylthio]-4H-pyrido[1,2-a]pyrimidin-4-oneAusbeute 16,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 2-mercapto-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (298 mg), 4,4'-bis(bromomethyl)benzophenone (934 mg), phenylpiperazine hydrochloride (402 mg) and potassium carbonate (850 mg) in DMF (30 ml) was stirred at room temperature for 10 hours. This reaction mixture was concentrated and the residue was dissolved in chloroform, washed with water, dried, and concentrated. The residue was purified by silica gel column chromatography (hexane: ethyl acetate =1:1) to provide the title compound as colorless solid (146 mg).

Aufarbeitung

  1. concentrationThis reaction mixture was concentrated
  2. dissolutionthe residue was dissolved in chloroform
  3. washwashed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (hexane: ethyl acetate =1:1)

Quellen und Nachweise

ORD-Eintrag
ord-53b480fb6d644aada34800c6e783f814
Quelldatensatz
uspto-grants-1998_05
Patentnummer
US05753664

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