Ethanol → 2-(3-Pyridyl)-6-(4-pyridyl)pyrimidin-4-one

HRID 853786

Reaktionsgleichung

Reaktionsgleichung von HRID 853786
[N:1]1[CH:6]=[CH:5][C:4]([C:7](=O)[CH2:8][C:9]([O:11]CC)=O)=[CH:3][CH:2]=1.Cl.[C:16]([C:19]1[CH:20]=[N:21][CH:22]=[CH:23][CH:24]=1)(=[NH:18])[NH2:17].C(=O)([O-])[O-].[K+].[K+].C(O)C>C(O)(=O)C>[N:21]1[CH:22]=[CH:23][CH:24]=[C:19]([C:16]2[NH:18][C:9](=[O:11])[CH:8]=[C:7]([C:4]3[CH:3]=[CH:2][N:1]=[CH:6][CH:5]=3)[N:17]=2)[CH:20]=1

Komponenten

6

Edukt 4

HCID 702EthanolHCID 11430Potassium CarbonateHCID 202042Nicotinamidine hydrochlorideHCID 2735202Ethyl 3-(4-pyridyl)-3-oxopropionate

Produkt 1

HCID 1354093932-(3-Pyridyl)-6-(4-pyridyl)pyrimidin-4-oneAusbeute 50,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
75 °C

Versuchsvorschrift

ethyl 3-(4-pyridyl)-3-oxopropionate (0.60 g), 3-amidinopyridine hydrochloride (0.54 g) and potassium carbonate (1.15 g) were added to 5 ml of ethanol, and the mixture was heated under reflux at 75° C. for 20 hours. Acetic acid was added to the reaction mixture, and the solvent was removed by distillation. The residue was added with water and then with acetic acid, and the resulting solid was separated by filtration, washed with water and ethyl acetate, and dried to obtain 0.39 g of the desired compound.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. customthe solvent was removed by distillation
  3. additionThe residue was added with water
  4. customwith acetic acid, and the resulting solid was separated by filtration
  5. washwashed with water and ethyl acetate
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-80f553bfe6ea4338b734b2fe6562c22a
Quelldatensatz
uspto-grants-2007_08
Patentnummer
US07256199B1

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