Potassium Carbonate → 2-[4-(4-hydroxybenzoyl)benzyloxy]-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one

HRID 1291393Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1291393
[OH: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].[Si]([O:21][C:22]1[CH:37]=[CH:36][C:25]([C:26]([C:28]2[CH:35]=[CH:34][C:31]([CH2:32]Br)=[CH:30][CH:29]=2)=[O:27])=[CH:24][CH:23]=1)(C(C)(C)C)(C)C.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[O:1][CH2:32][C:31]1[CH:30]=[CH:29][C:28]([C:26](=[O:27])[C:25]2[CH:36]=[CH:37][C:22]([OH:21])=[CH:23][CH:24]=2)=[CH:35][CH:34]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 18918912HCID 18918912, VerbindungHCID 135448456HCID 135448456, Verbindung

Produkt 1

HCID 189188752-[4-(4-hydroxybenzoyl)benzyloxy]-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-oneAusbeute 4,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 2-hydroxy-3-methyl-4H-pyrido[1,2-a]pyrimidin-4-one (3.158 g), 4-(4-t-butyldimethylsilyloxybenzoyl)benzyl bromide (12.24 g) and potassium carbonate (5.07 g) in DMF (50 ml) was stirred at room temperature for 24 hours. This reaction mixture was concentrated and the residue was purified by silica gel column chromatography (dichloromethane: ethyl acetate =1:2) and recrystallized from chloroform-methanol-ethyl acetate to provide the title compound as colorless solid (325 mg).

Aufarbeitung

  1. concentrationThis reaction mixture was concentrated
  2. customthe residue was purified by silica gel column chromatography (dichloromethane: ethyl acetate =1:2)
  3. customrecrystallized from chloroform-methanol-ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-2e836f995f4b49089e9108168dc40fae
Quelldatensatz
uspto-grants-1998_05
Patentnummer
US05753664

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