Reaktion #11603

ord-4617c2c237a047b3afb73ffa4846eb05

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    FiltrationThe reaction mixture is filtered through celite
  2. 2
    Sonstigeto remove the Raney nickel
  3. 3
    EinengenThe filtrate is concentrated under reduced pressure

Vorschrift

A solution of diethyl-[3-(4-nitro-phenoxy)-propyl]-amine (15.2 g, 60.4 mmol) is dissolved in absolute ethanol (350 mL) and to this solution is added hydrazine monohydrate (18 mL, 6 equiv.) followed by the addition of a small portion of Raney nickel. The reaction mixture is heated to 50° C. with stirring for 3 h until all gas evolution has ceased. The reaction mixture is filtered through celite to remove the Raney nickel. The filtrate is concentrated under reduced pressure to give the named compound as a greenish brown oil (quantitative). This material is carried on in subsequent steps without purification.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07098236B2uspto-grants-2006_08