Reaktion #47992

ord-d086c88d01994e01b7fbf7faf0ac7880

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe reaction is heated
  2. 2
    Temperaturto reflux for 4 hours
  3. 3
    Filtrationfiltered through a Celite™
  4. 4
    Filtrationfilter
  5. 5
    SonstigeEvaporation

Vorschrift

2,2′,4-Trimethoxybenzophenone oxime (6 g, 20.9 mmol) is dissolved in ethanol (30 ml) and concentrated aqueous ammonia (150 ml). Ammonium acetate (0.81 g, 10.45 mmol) is added, followed by zinc powder (6.79 g, 104 mmol). The reaction is heated to reflux for 4 hours, cooled to ambient temperature, diluted with ethyl acetate and filtered through a Celite™ filter. Evaporation affords the title compound. δH 3.78 (s 3H), 3.80 (s 3H), 3.82 (s 3H), 5.62 (s 3H), 6.40-6.50 (m 2H), 6.85-9.95 (m 2H), 7.10 (d J 8), 7.20-7.30 (m 2H)

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07745462B2uspto-grants-2010_06