Sodium Thiosulfate → 5-Chloro-2-methylpyridazin-3(2H)-one

HRID 237595Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 237595
Cl[C:2]1[C:3](=[O:10])[N:4]([CH3:9])[N:5]=[CH:6][C:7]=1[Cl:8].[O-]S([O-])(=S)=O.[Na+].[Na+]>I>[Cl:8][C:7]1[CH:6]=[N:5][N:4]([CH3:9])[C:3](=[O:10])[CH:2]=1

Komponenten

4

Edukt 2

HCID 24477Sodium ThiosulfateHCID 1204623(2H)-Pyridazinone, 4,5-dichloro-2-methyl-

Produkt 1

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

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 24841Hydrogen iodideLösungsmittel

Versuchsvorschrift

4,5-Dichloro-2-methylpyridazin-3(2H)-one (1 g) is dissolved in aqueous HI solution (57%, 8.5 mL) and the mixture is heated to reflux for 12 hours. After cooling to room temperature the mixture is treated with aqueous Na2S2O3 solution (30%, 100 mL) and stirred for 1 hour. The mixture is then extracted three times with dichloromethane. The combined organic phases are washed with brine, dried (MgSO4) and concentrated. The residue is triturated with diisopropylether. Yield: 414 mg; Mass spectrum (ESI+): m/z=145 [M+H]+.

Aufarbeitung

  1. temperaturethe mixture is heated
  2. temperatureto reflux for 12 hours
  3. extractionThe mixture is then extracted three times with dichloromethane
  4. washThe combined organic phases are washed with brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated
  7. customThe residue is triturated with diisopropylether

Quellen und Nachweise

ORD-Eintrag
ord-bc315bb3740a49ddafbcfe3f4996b634
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08642585B2

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