Reaktion #64266
ord-6fe17835193343a7a4500ca2f185301b
Reaktionsgleichung
Reagenzien
Keine
Reaktionsbedingungen
Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1SonstigeIn a 250 mL flask equipped with a nitrogen inlet
- 2Temperaturreflux condenser
- 3Temperaturcooled to room temperature
- 4workup.STIRRINGstirred for an additional 16 h
- 5Extraktionthe organics were extracted
- 6Trocknendried over magnesium sulfate
- 7Sonstigethe solvents were removed under reduced pressure
- 8Sonstigeto yield a yellow powder
- 9SonstigeRecrystallization 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##