反应 #42735

反应方程式

2,3-difluorophenol

aluminium chloride

(4-chlorophenyl)acetyl chloride

→

title compound

2-(4-Chlorophenyl)-1-(3,4-difluoro-2-hydroxy-phenyl)-ethanone

溶剂

1,2-dichloroethane

1,2-dichloroethane

water

反应条件

后处理

1. 1
   温度is heated in an oil bath at 90° C. overnight
2. 2
   温度The reaction mixture is cooled to room temperature
3. 3
   萃取extracted with ethyl acetate
4. 4
   干燥The organic phase is dried over anhydrous magnesium sulfate
5. 5
   过滤filtered
6. 6
   其他evaporated to dryness in vacuo
7. 7
   其他to afford a brown solid
8. 8
   其他This is triturated with hexane/ethyl acetate (9:1)
9. 9
   过滤filtered
10. 10
    其他dried

实验过程

A mixture of aluminium chloride (7.66 g, 57.4 mmol, 1.5 eq.) and (4-chlorophenyl)acetyl chloride (8.7 g, 46 mmol, 1.2 eq.) in 1,2-dichloroethane (75 ml) is stirred at 0° C. for 30 min. A solution of 2,3-difluorophenol (5 g, 38.4 mmol) in 1,2-dichloroethane (25 ml) is added to the reaction mixture, which is heated in an oil bath at 90° C. overnight. The reaction mixture is cooled to room temperature, diluted with water and extracted with ethyl acetate. The organic phase is dried over anhydrous magnesium sulfate, filtered and evaporated to dryness in vacuo to afford a brown solid. This is triturated with hexane/ethyl acetate (9:1), filtered and dried to afford the title compound as a pale brown fine solid which is 87% pure by HPLC analysis.

来源