Sodium Carbonate → HCID 15951413, Verbindung

HRID 271114Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 271114
[C:1]1([C:7](=O)[C:8]([C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)=O)[CH:6]=[CH:5][CH:4]=[CH:3]C=1.Cl.[CH3:18][NH:19][C:20]([NH2:22])=[NH:21].[C:23]([O-:26])([O-])=O.[Na+].[Na+]>CCO.O>[NH2:22][C:20]1[N:19]([CH3:18])[C:23](=[O:26])[C:8]([C:7]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:1]=2)([C:10]2[CH:11]=[CH:12][N:13]=[CH:14][CH:15]=2)[N:21]=1

Komponenten

6

Edukt 3

HCID 10340Sodium CarbonateHCID 2750111-Phenyl-2-pyridin-4-ylethane-1,2-dioneHCID 178485118HCID 178485118, Verbindung

Produkt 1

HCID 15951413HCID 15951413, VerbindungAusbeute 62 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel2×

Versuchsvorschrift

A suspension of 1-phenyl-2-pyridin-4-ylethane-1,2-dione (0.81 g, 3.8 mmol), N-methylguanidine hydrochloride (1.92 g, 17.5 mmol) and Na2CO3 (3.71 g, 35 mmol) in EtOH (25 mL) and H2O (5 mL) is refluxed for 18 h. The reaction mixture is cooled and poured into water. The precipitate is collected by filtration, washed with water, and air-dried to give the title compound (0.62 g, 62%) as a solid. Mp 154-155° C. MS (+) ES: 267 (M+H)+.

Aufarbeitung

  1. temperatureis refluxed for 18 h
  2. temperatureThe reaction mixture is cooled
  3. filtrationThe precipitate is collected by filtration
  4. washwashed with water
  5. customair-dried

Quellen und Nachweise

ORD-Eintrag
ord-706075c3babf4dd684bd9f7557cabc6a
Quelldatensatz
uspto-grants-2008_11
Patentnummer
US07452885B2

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