Cyclopropylamine → 4,5-Dichloro-2-cyclopropylaminobenzenesulphonamide

HRID 17835

Reaktionsgleichung

Reaktionsgleichung von HRID 17835
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([S:9]([NH2:12])(=[O:11])=[O:10])=[C:4](F)[CH:3]=1.[CH:14]1([NH2:17])[CH2:16][CH2:15]1>O1CCOCC1>[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5]([S:9]([NH2:12])(=[O:11])=[O:10])=[C:4]([NH:17][CH:14]2[CH2:16][CH2:15]2)[CH:3]=1

Komponenten

4

Edukt 2

HCID 69828CyclopropylamineHCID 675307044,5-Dichloro-2-fluorobenzenesulfonamide

Produkt 1

HCID 675298334,5-Dichloro-2-cyclopropylaminobenzenesulphonamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
105 °C

Versuchsvorschrift

A solution of 4,5-dichloro-2-fluorobenzenesulphonamide (3 g) in dioxane (30 mL) to which cyclopropylamine (3 mL) has been added is heated at 100-110° C. in a hermetically closed vessel for 24 hours. The solvent and the excess of amine are removed by distillation under reduced pressure and the residue is dissolved in methanol (20 mL). The methanolic solution is cooled on an ice bath, and water (60 mL) is added. The precipitate obtained (the title product) is collected by filtration, washed with water and dried. It is used in the following Step without being otherwise purified.

Aufarbeitung

  1. customThe solvent and the excess of amine are removed by distillation under reduced pressure
  2. dissolutionthe residue is dissolved in methanol (20 mL)
  3. temperatureThe methanolic solution is cooled on an ice bath
  4. additionwater (60 mL) is added

Quellen und Nachweise

ORD-Eintrag
ord-8df3b2af4ad44a3c9cd5221054a83a8f
Quelldatensatz
uspto-grants-2010_06
Patentnummer
US07741320B2

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