反应详情

温度

100 °C

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##

1. customIn a 250 mL flask equipped with a nitrogen inlet
2. temperaturereflux condenser
3. temperaturecooled to room temperature
4. stirringstirred for an additional 16 h
5. extractionthe organics were extracted
6. dry with materialdried over magnesium sulfate
7. customthe solvents were removed under reduced pressure
8. customto yield a yellow powder
9. customRecrystallization from acetone