Nitric Acid → 2,5-Dichloro-4-nitrothiophene-3-sulfonyl chloride

HRID 1973155Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1973155
[Cl:1][C:2]1[S:3][C:4]([Cl:11])=[CH:5][C:6]=1[S:7]([Cl:10])(=[O:9])=[O:8].[N+:12]([O-])([OH:14])=[O:13]>S(=O)(=O)(O)O>[Cl:1][C:2]1[S:3][C:4]([Cl:11])=[C:5]([N+:12]([O-:14])=[O:13])[C:6]=1[S:7]([Cl:10])(=[O:8])=[O:9]

Komponenten

4

Edukt 2

HCID 944Nitric AcidHCID 27360942,5-Dichlorothiophene-3-sulfonyl chloride

Produkt 1

HCID 27772072,5-Dichloro-4-nitrothiophene-3-sulfonyl chloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1118Sulfuric AcidLösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

A 55.8-g (0.22 mol) sample of 2,5-dichloro-3-thienylsulfonyl chloride was added in small portions to a stirred solution of 150 ml concentrated nitric acid and 150 ml concentrated sulfuric acid. After the addition was completed, the reaction mixture was stirred at about 25° C overnight. The reaction mixture was then diluted with ice water and filtered to give the crude 2,5-dichloro-4-nitro-3-thienylsulfonyl chloride product. The product was washed with water and dried. Recrystallization from methylene chloride gave the product as a brown solid, m.p. 89°-91° C.

Aufarbeitung

  1. additionAfter the addition
  2. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-d7f6788cfa0640dcbfeebb68bf95144c
Quelldatensatz
uspto-grants-1976_12
Patentnummer
US03996243

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