Aniline → Phenylsulfamoyl chloride

HRID 1070739Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1070739
[Cl:1][S:2]([OH:5])(=O)=[O:3].[NH2:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C(Cl)Cl>[C:7]1([NH:6][S:2]([Cl:1])(=[O:5])=[O:3])[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1

Komponenten

4

Edukt 2

HCID 6115AnilineHCID 24638Chlorosulfonic acid

Produkt 1

HCID 11564615Phenylsulfamoyl chloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
-5 °C

Versuchsvorschrift

25.2 g of chlorosulphonic acid are added slowly to a solution of 60.6 g of aniline in 316 ml of methylene chloride cooled to −5° C. When the addition is complete, the mixture is allowed to return to ambient temperature and the precipitate obtained is filtered off. After drying, the precipitate is taken up in 231 ml of toluene, and 45.1 g of phosphorus pentachloride are added gradually. The mixture is then refluxed for 3 hours 30 minutes and, after returning to ambient temperature, the precipitate formed is filtered off. The filtrate is concentrated to obtain the expected product.

Aufarbeitung

  1. additionWhen the addition
  2. customto return to ambient temperature
  3. customthe precipitate obtained
  4. filtrationis filtered off
  5. customAfter drying
  6. addition45.1 g of phosphorus pentachloride are added gradually
  7. temperatureThe mixture is then refluxed for 3 hours 30 minutes
  8. customafter returning to ambient temperature
  9. customthe precipitate formed
  10. filtrationis filtered off
  11. concentrationThe filtrate is concentrated

Quellen und Nachweise

ORD-Eintrag
ord-c4910a47f5eb4f3fa49d4f0043221342
Quelldatensatz
uspto-grants-2005_06
Patentnummer
US06903103B2

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