Reaktion #46116

ord-cc7cdf4d90fc4c72980716ddfe9808c6

Reaktionsgleichung

NS(=O)(=O)c1cc([N+](=O)[O-])ccc1Cl
2-Chloro-5-nitrobenzenesulphonamide
NC1CC1
cyclopropylamine
NS(=O)(=O)c1cc([N+](=O)[O-])ccc1NC1CC1
2-cyclopropylamino-5-nitrobenzenesulphonamide

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONabove is introduced into a hermetically closed vessel
  2. 2
    workup.ADDITIONcontaining
  3. 3
    SonstigeAfter this time period, the solvent and the reagent are removed
  4. 4
    Einengenby concentrating under reduced pressure
  5. 5
    Filtrationis collected by filtration
  6. 6
    Waschenwashed with methanol
  7. 7
    Sonstigedried

Vorschrift

2-Chloro-5-nitrobenzenesulphonamide (5 g) prepared in the Step above is introduced into a hermetically closed vessel containing a mixture of dioxane (70 mL) and cyclopropylamine (3.5 mL). The hermetically closed vessel is placed in an oven at 100° C. for 24 hours. After this time period, the solvent and the reagent are removed by concentrating under reduced pressure. The residue is taken up in methanol (20 mL) and the insoluble material, which contains the title product, is collected by filtration, washed with methanol and dried.

Quelle

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