Hydrochloric Acid → 5-Bromopyridine-3-sulphonic acid

HRID 839386Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 839386
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([S:7]([OH:10])(=[O:9])=[O:8])[CH:2]=1.P(Cl)(Cl)(Cl)(Cl)Cl.Cl.[Br:18]Br>O.C(Cl)(Cl)Cl>[Br:18][C:5]1[CH:4]=[C:3]([S:7]([OH:10])(=[O:9])=[O:8])[CH:2]=[N:1][CH:6]=1

Komponenten

7

Edukt 4

HCID 313Hydrochloric AcidHCID 24408BromineHCID 24819Phosphorus pentachlorideHCID 694683-Pyridinesulfonic acid

Produkt 1

HCID 126842615-Bromopyridine-3-sulphonic acid

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6212ChloroformLösungsmittel

Versuchsvorschrift

A mixture of 3g. of 3-pyridinesulfonic acid and 8.5g. of phosphorous pentachloride was heated at 120° C for 1.5 hours. Upon cooling to room temperature, the mixture solidified. Chloroform was added thereto and dry hydrogen chloride gas was introduced. The resulting precipitate was collected by filtration and dried. The crystalline substance obtained was heated with bromine (4g.) at 120° C. for 8 hours and water (60 ml.) was added to the mixture. After stirring at 80° C. for 2 hours, the solution was concentrated. On addition of acetone, 2g. of 5-bromo- 3-pyridinesulfonic acid was obtained.

Aufarbeitung

  1. filtrationThe resulting precipitate was collected by filtration
  2. customdried
  3. customThe crystalline substance obtained
  4. concentrationthe solution was concentrated
  5. additionOn addition of acetone, 2g

Quellen und Nachweise

ORD-Eintrag
ord-fe469ed7e841436a912cd1202abd0cfd
Quelldatensatz
uspto-grants-1978_06
Patentnummer
US04094982

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