Reaktion #64266

ord-6fe17835193343a7a4500ca2f185301b

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeIn a 250 mL flask equipped with a nitrogen inlet
  2. 2
    Temperaturreflux condenser
  3. 3
    Temperaturcooled to room temperature
  4. 4
    workup.STIRRINGstirred for an additional 16 h
  5. 5
    Extraktionthe organics were extracted
  6. 6
    Trocknendried over magnesium sulfate
  7. 7
    Sonstigethe solvents were removed under reduced pressure
  8. 8
    Sonstigeto yield a yellow powder
  9. 9
    SonstigeRecrystallization from acetone

Vorschrift

In a 250 mL flask equipped with a nitrogen inlet, overhead stirring assembly, and reflux condenser were placed 4-nitrobenzoyl chloride (22.6 g, 0.122 mol), bromobenzene (100 g, 0.63 mol), and aluminum chloride (17.3 g, 0.13 mol). The mixture was heated for 3 h at 100° C., then cooled to room temperature and stirred for an additional 16 h. The mixture was poured into 1 L of acidic (HCl) ice water, and the organics were extracted using methylene chloride, dried over magnesium sulfate, and the solvents were removed under reduced pressure to yield a yellow powder. Recrystallization from acetone afforded 29.2 g (85% yield) of yellow crystals: m.p. 123°-124° C., (Lit. 122° C.). ##STR5##

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05412066uspto-grants-1995_05