Reaktion #46113

ord-8df3b2af4ad44a3c9cd5221054a83a8f

Reaktionsgleichung

NS(=O)(=O)c1cc(Cl)c(Cl)cc1F
4,5-dichloro-2-fluorobenzenesulphonamide
NC1CC1
cyclopropylamine
NS(=O)(=O)c1cc(Cl)c(Cl)cc1NC1CC1
title product
NS(=O)(=O)c1cc(Cl)c(Cl)cc1NC1CC1
4,5-dichloro-2-cyclopropylaminobenzenesulphonamide

Lösungsmittel

Reaktionsbedingungen

Temperatur
105°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

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

Vorschrift

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.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07741320B2uspto-grants-2010_06