2,5-Dichlorobenzenesulfonamide → 2-Mercapto-5-Chloro-benzenesulfonamide

HRID 583480Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 583480
Cl[C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[S:9]([NH2:12])(=[O:11])=[O:10].[SH2:13].[Na]>CN(C=O)C>[SH:13][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[S:9]([NH2:12])(=[O:11])=[O:10]

Komponenten

4

Edukt 2

HCID 2380452,5-DichlorobenzenesulfonamideHCID 86586439Sodium hydrogen sulphide

Produkt 1

HCID 189353412-Mercapto-5-Chloro-benzenesulfonamideAusbeute 30,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To 34.0 g (0.15 mol) of 2,5-dichloro-benzene sulfonamide in 200 mL of DMF was added 16.0 g (0.28 mol) of sodium hydrogensulfide. The mixture was refluxed for 18 hours, then cooled, concentrated, and the solids collected by filtration. The solids were dissolved in hot water, the pH adjusted to 4.0 and the precipitate filtered. This material was dried to yield 10.1 g of the title compound, mp 142-144° C.

Aufarbeitung

  1. temperatureThe mixture was refluxed for 18 hours
  2. temperaturecooled
  3. concentrationconcentrated
  4. filtrationthe solids collected by filtration
  5. dissolutionThe solids were dissolved in hot water
  6. filtrationthe precipitate filtered
  7. customThis material was dried

Quellen und Nachweise

ORD-Eintrag
ord-28e1896881ee49b7a24cbcab721e78b9
Quelldatensatz
uspto-grants-1999_07
Patentnummer
US05929114

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