反应 #607494

反应方程式

aluminum trichloride

DCE

144b

4-bromo-2-fluorobenzoyl chloride

DCE

→

1-(4-bromo-2-fluorophenyl)-3-chloropropan-1-one

收率 68.0%

反应条件

后处理

1. 1
   其他Ethylene gas was bubbled through the dark suspension for 3 h until the acid chloride
2. 2
   其他was consumed
3. 3
   温度cooled to 0° C.
4. 4
   其他quenched with 4M HCl (500 mL)
5. 5
   其他The organic phase was separated
6. 6
   洗涤washed with brine (100 mL)
7. 7
   干燥dried over anhydrous sodium sulfate
8. 8
   浓缩concentrated under reduced pressure
9. 9
   其他The crude residue was purified by column chromatography (PE/EA=30 to 10:1)

实验过程

To a stirred suspension of aluminum trichloride (153 g, 1.15 mol) in DCE (1000 mL) was added a solution of 144b (271 g, 1.14 mol) in DCE (1000 mL) at 0° C. See FIG. 3. Ethylene gas was bubbled through the dark suspension for 3 h until the acid chloride was consumed. The reaction mixture was then stirred at RT overnight, cooled to 0° C., and quenched with 4M HCl (500 mL). The organic phase was separated and washed with brine (100 mL), dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The crude residue was purified by column chromatography (PE/EA=30 to 10:1) to give 1-(4-bromo-2-fluorophenyl)-3-chloropropan-1-one 144c (210 g, 68%).

来源