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

HRID 1524520
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1524520
[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-2a4c6fcd11624d588d842a8da755c32f
Quelldatensatz
uspto-grants-2015_07
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09079906B2

Notizen zur Reaktion

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