Reaktion #66151

ord-5d8f74c42ce14871b154b69129200291

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction mixture was heated
  2. 2
    Temperaturto reflux for 15 hours
  3. 3
    Filtrationfiltered
  4. 4
    EinengenThe filtrate was concentrated under reduced pressure

Vorschrift

To a solution of 1-(4,6-dimethyl-pyridin-2-yl)-4-(4-nitro-phenyl)-[1,4]diazepane (940 mg, 2.88 mmol) in ethyl acetate (25 mL) was added stannous chloride (3.90 g, 17.3 mmol) and ethanol (5 mL). The reaction mixture was heated to reflux for 15 hours then cooled to room temperature, basified with triethylamine and filtered. The filtrate was concentrated under reduced pressure to afford 4-[4-(4,6-dimethyl-pyridin-2-yl)-[1,4]diazepan-1-yl]-phenylamine (850 mg, 99%) as a brown solid.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08524705B2uspto-grants-2013_09