Benzenesulfonyl chloride, 4-chloro-3-nitro- → 3-amino-4-chlorobenzenethiol

HRID 1512972Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1512972
[Sn].[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([S:9](Cl)(=O)=O)=[CH:5][C:4]=1[N+:13]([O-])=O>Cl>[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([SH:9])=[CH:5][C:4]=1[NH2:13]

Komponenten

4

Edukt 2

HCID 7323Benzenesulfonyl chloride, 4-chloro-3-nitro-HCID 5352426Tin atom

Produkt 1

HCID 6406993-amino-4-chlorobenzenethiolAusbeute 73,9 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

To a mixture of concentrated hydrochloric acid (30 mL) and ice (25 g) was added tin (29.7 g) under ice-cooling, followed by adding 4-chloro-3-nitrobenzenesulfonyl chloride (6.4 g), and the mixture was stirred under ice-cooling for 1.5 hours, and then stirred at 90° C. for 2 hours. The insoluble material was removed by filtration, and the filtrate was stirred at room temperature overnight. The precipitated crystals were collected by filtration. The collected crystals were washed with water, and dried under reduced pressure to give the title compound (2.95 g).

Aufarbeitung

  1. temperaturecooling
  2. temperaturecooling for 1.5 hours
  3. stirringstirred at 90° C. for 2 hours
  4. customThe insoluble material was removed by filtration
  5. stirringthe filtrate was stirred at room temperature overnight
  6. filtrationThe precipitated crystals were collected by filtration
  7. washThe collected crystals were washed with water
  8. customdried under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-53fa4a2a38bf49118caa5aeffe7e6413
Quelldatensatz
uspto-grants-2012_07
Patentnummer
US08217069B2

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