Réaction #64266
ord-6fe17835193343a7a4500ca2f185301b
Équation de réaction
Réactifs
Aucun
Conditions de réaction
Température
100°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.
Traitement
- 1AutreIn a 250 mL flask equipped with a nitrogen inlet
- 2Températurereflux condenser
- 3Températurecooled to room temperature
- 4workup.STIRRINGstirred for an additional 16 h
- 5Extractionthe organics were extracted
- 6Séchagedried over magnesium sulfate
- 7Autrethe solvents were removed under reduced pressure
- 8Autreto yield a yellow powder
- 9AutreRecrystallization from acetone
Mode opératoire
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##