Reaktion #53198

ord-0770d44e24ec4c24a921ae9eccf562c9

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturwhile cooling with ice
  2. 2
    Sonstigeto come up slowly to ambient temperature
  3. 3
    Waschenthe mixture is washed with dichloromethane
  4. 4
    Extraktionthe product is extracted with dichloromethane

Vorschrift

2.7 g (86 mmol) of methylamine are dissolved in 120 ml of dichloromethane while cooling with ice. 4.9 g (21 mmol) of 4-(2-bromoethyl)-nitrobenzene are added and the mixture is allowed to come up slowly to ambient temperature. After 15 hours stirring the solvent is eliminated in vacuo and the residue taken up in water. An acid pH is created using 2 N hydrochloric acid and the mixture is washed with dichloromethane. The aqueous phase is then adjusted to a basic pH using 4 N sodium hydroxide solution and the product is extracted with dichloromethane.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06855710B2uspto-grants-2005_02