Methyl iodide → 6-chloro-2-methyl[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one

HRID 397572

Reaktionsgleichung

Reaktionsgleichung von HRID 397572
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8](=[O:11])[NH:9][N:10]=2)[N:7]=1.[C:12](=O)([O-])[O-].[K+].[K+].CI>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([C:8](=[O:11])[N:9]([CH3:12])[N:10]=2)[N:7]=1

Komponenten

5

Edukt 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 64071826-chloro-2H,3H-[1,2,4]triazolo[4,3-b]pyridazin-3-one

Produkt 1

HCID 230003286-chloro-2-methyl[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-oneAusbeute 67,2 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

0.853 g of 6-chloro[1,2,4]triazolo[4,3-b]pyridazin-3(2H)-one was dissolved in 5 ml of N,N-dimethylformamide; 0.83 g of potassium carbonate was added; with stirring at room temperature, 0.5 ml of methyl iodide was added. After stirring at room temperature for 15 hours, ice water and saline were added; the reaction mixture was extracted with ethyl acetate-tetrahydrofuran (1:1); the extract was washed with saline and dried over magnesium sulfate. After concentration under reduced pressure, the crystal obtained was collected by filtration, washed with diethyl ether, and dried, to yield 0.62 g of the title compound.

Aufarbeitung

  1. stirringAfter stirring at room temperature for 15 hours
  2. extractionthe reaction mixture was extracted with ethyl acetate-tetrahydrofuran (1:1)
  3. washthe extract was washed with saline
  4. dry with materialdried over magnesium sulfate
  5. concentrationAfter concentration under reduced pressure
  6. customthe crystal obtained
  7. filtrationwas collected by filtration
  8. washwashed with diethyl ether
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-809f861659cd41a7b0f787210052c141
Quelldatensatz
uspto-grants-2003_08
Patentnummer
US06610694B1

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