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3,4,6-Trichloropyridazine → 3,6-Dichloro-4-methanesulfonylpyridazine

HRID 657927
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 657927
[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1Cl.[Na+].[CH3:11][S:12]([O-:14])=[O:13]>O.C1COCC1.CN(C=O)C>[Cl:1][C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[S:12]([CH3:11])(=[O:14])=[O:13]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 951233,4,6-TrichloropyridazineHCID 2733271Sodium methanesulfinate

Produkt 1

HCID 580457893,6-Dichloro-4-methanesulfonylpyridazine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 86606902water THF DMFLösungsmittel

Versuchsvorschrift

3,4,6-Trichloropyridazine (2.5 g; 13.6 mmol) and methanesulfinic acid sodium salt (2.78 g, 27.26 mmol) were stirred in 20 ml of a solvent mixture of water/THF/DMF (5:10:5) at RT for 30 h. The solvent was removed under reduced pressure and the residue was partitioned between ethyl acetate and saturated ammonium chloride solution. The organic phase was removed and concentrated, and the crude product was purified by flash chromatography (dichloromethane:methanol). Yield: 1.4 g

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Aufarbeitung

  1. customThe solvent was removed under reduced pressure
  2. customthe residue was partitioned between ethyl acetate and saturated ammonium chloride solution
  3. customThe organic phase was removed
  4. concentrationconcentrated
  5. customthe crude product was purified by flash chromatography (dichloromethane:methanol)

Quellen und Nachweise

ORD-Eintrag
ord-f3c01bf9600a496c89aa13cb31eb9f0c
Quelldatensatz
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08076336B2

Notizen zur Reaktion

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