反应 #64267

反应方程式

HCl

fluorobenzene

4-bromobenzoyl chloride

aluminum chloride

→

4-bromo-4'-fluorobenzophenone

收率 86.0%

反应条件

后处理

1. 1
   其他In a 250 mL flask equipped with a nitrogen inlet
2. 2
   温度reflux condenser
3. 3
   workup.STIRRINGThe mixture was stirred for 15 minutes at 23° C.
4. 4
   温度by heating
5. 5
   温度to reflux for 4 h
6. 6
   温度The reaction was then cooled to 23° C.
7. 7
   workup.STIRRINGstirred for 16 h
8. 8
   萃取The organics were extracted with methylene chloride
9. 9
   干燥dried over magnesium sulfate
10. 10
    过滤The slurry was filtered
11. 11
    其他the methylene chloride was removed under reduced pressure
12. 12
    其他to yield an off white powder
13. 13
    其他Recrystallization from ethanol

实验过程

In a 250 mL flask equipped with a nitrogen inlet, overhead stirring assembly, and reflux condenser were placed fluorobenzene (117 g, 1.2 mol) and 4-bromobenzoyl chloride (39.8 g, 0.181 mol). The mixture was cooled to 0° C. and aluminum chloride (27 g, 0.20 mol) was added. The mixture was stirred for 15 minutes at 23° C., followed by heating to reflux for 4 h. The reaction was then cooled to 23° C. and stirred for 16 h. The resulting slurry was poured into 2 L of acidic (HCl) water. The organics were extracted with methylene chloride, and dried over magnesium sulfate. The slurry was filtered and the methylene chloride was removed under reduced pressure to yield an off white powder. Recrystallization from ethanol afforded 43.3 g (86%) of 4-bromo-4'-fluorobenzophenone as white crystals: m.p. 106°-107° C., (Lit. 107°-108° C.).

来源