Ethanol → 1-Methyl-4-(4-methyl-5-methylsulfanyl-4h-[1,2,4]triazol-3-yl)-1h-pyridin-2-one

HRID 500552Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 500552
[SH:1][C:2]1[N:3]([CH3:15])[C:4]([C:7]2[CH:12]=[CH:11][N:10]([CH3:13])[C:9](=[O:14])[CH:8]=2)=[N:5][N:6]=1.[OH-].[Na+].[CH2:18](O)C.IC>O>[CH3:13][N:10]1[CH:11]=[CH:12][C:7]([C:4]2[N:3]([CH3:15])[C:2]([S:1][CH3:18])=[N:6][N:5]=2)=[CH:8][C:9]1=[O:14]

Komponenten

6

Edukt 4

HCID 702EthanolHCID 6328Methyl iodideHCID 14798Sodium HydroxideHCID 178481695HCID 178481695, Verbindung

Produkt 1

HCID 248520611-Methyl-4-(4-methyl-5-methylsulfanyl-4h-[1,2,4]triazol-3-yl)-1h-pyridin-2-oneAusbeute 78 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel2×

Versuchsvorschrift

The title compound from example 32.1 (600 mg, 2.7 mmol) was dissolved in a solution of sodium hydroxide (216 mg, 5.4 mmol) and water (5 mL). When a clear, uniform solution was observed ethanol (6 mL) was added, followed by iodomethane (268 μL, 4.3 mmol). The reaction was stirred at room temperature for 6 h. The reaction mixture was then diluted with water and extracted four times with chloroform. The organic phase was dried over magnesium sulfate, filtered and concentrated to yield the title compound (yellowish solid, 500 mg, 78%).

Aufarbeitung

  1. additionwas added
  2. extractionextracted four times with chloroform
  3. dry with materialThe organic phase was dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-21cd996aec87452e82cc17978abd2a69
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07772235B2

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