Methyl iodide → 5-Chloro-2-methylpyridazin-3(2H)-one

HRID 57850

Reaktionsgleichung

Reaktionsgleichung von HRID 57850
[Cl:1][C:2]1[CH:3]=[N:4][NH:5][C:6](=[O:8])[CH:7]=1.IC.[C:11](=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[N:4][N:5]([CH3:11])[C:6](=[O:8])[CH:7]=1

Komponenten

5

Edukt 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 199057185-Chloropyridazin-3(2H)-one

Produkt 1

HCID 129101445-Chloro-2-methylpyridazin-3(2H)-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A solution of 4-chloro-1H-pyridazin-6-one (6.000 mmol; 783.2 mg), Iodomethane (7.200 mmol; 1032 mg; 0.453 mL), and potassium carbonate (9.000 mmol; 1256 mg) in DMF (12 mL) was stirred at room temperature overnight. The mixture was filtered. The filtrate was partitioned between EtOAc and water. The organic layer was concentrated. The residue was purified on silica eluted with 0 to 40% EtOAc in DCM to afford 5-chloro-2-methyl-pyridazin-3-one as an off-white solid (514.7, 59%).

Aufarbeitung

  1. filtrationThe mixture was filtered
  2. customThe filtrate was partitioned between EtOAc and water
  3. concentrationThe organic layer was concentrated
  4. customThe residue was purified on silica
  5. washeluted with 0 to 40% EtOAc in DCM

Quellen und Nachweise

ORD-Eintrag
ord-629f6a2a648d414ab2141a7d9626c816
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09434725B2

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