Methyl iodide → 2-Methoxy-4-(4-methyl-5-methylsulfanyl-4h-[1,2,4]triazol-3-yl)-pyridine

HRID 500545Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 500545
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]2[N:10]([CH3:15])[C:11]([SH:14])=[N:12][N:13]=2)[CH:6]=[CH:5][N:4]=1.I[CH3:17]>[OH-].[Na+].C(O)C>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]2[N:10]([CH3:15])[C:11]([S:14][CH3:17])=[N:12][N:13]=2)[CH:6]=[CH:5][N:4]=1

Komponenten

5

Edukt 2

HCID 6328Methyl iodideHCID 178488243HCID 178488243, Verbindung

Produkt 1

HCID 248517082-Methoxy-4-(4-methyl-5-methylsulfanyl-4h-[1,2,4]triazol-3-yl)-pyridineAusbeute 97,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 14798Sodium HydroxideLösungsmittel

Versuchsvorschrift

The title compound of example 24.1 (21.30 g, 95.83 mmol) was set stirring in 1 M sodium hydroxide in a cold water bath. Iodomethane (21.76 g, 153.3 mmol) in ethanol (63 mL) was added to the reaction. As the reaction progressed, solid began to precipitate out. The reaction was allowed to stir at RT for 12 hours. The reaction mixture was extracted with dichloromethane and the organic extracts were washed with brine, dried and concentrated to afford the title compound as a white solid (22 g, 97%).

Aufarbeitung

  1. customto precipitate out
  2. extractionThe reaction mixture was extracted with dichloromethane
  3. washthe organic extracts were washed with brine
  4. customdried
  5. concentrationconcentrated

Quellen und Nachweise

ORD-Eintrag
ord-61e32176a0d44470aed2709f2325e35b
Quelldatensatz
uspto-grants-2010_08
Patentnummer
US07772235B2

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