反応 #64266

反応方程式

HCl

4-nitrobenzoyl chloride

bromobenzene

aluminum chloride

→

yellow crystals

収率 85.0%

4-bromo-4'-nitrobenzophenone

収率 85.0%

反応条件

後処理

1. 1
   その他In a 250 mL flask equipped with a nitrogen inlet
2. 2
   温度reflux condenser
3. 3
   温度cooled to room temperature
4. 4
   workup.STIRRINGstirred for an additional 16 h
5. 5
   抽出the organics were extracted
6. 6
   乾燥dried over magnesium sulfate
7. 7
   その他the solvents were removed under reduced pressure
8. 8
   その他to yield a yellow powder
9. 9
   その他Recrystallization from acetone

実験手順

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##

出典