反応 #42735

反応方程式

2,3-difluorophenol

aluminium chloride

(4-chlorophenyl)acetyl chloride

→

title compound

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

溶媒

1,2-dichloroethane

1,2-dichloroethane

water

反応条件

後処理

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
   抽出extracted with ethyl acetate
4. 4
   乾燥The organic phase is dried over anhydrous magnesium sulfate
5. 5
   ろ過filtered
6. 6
   その他evaporated to dryness in vacuo
7. 7
   その他to afford a brown solid
8. 8
   その他This is triturated with hexane/ethyl acetate (9:1)
9. 9
   ろ過filtered
10. 10
    その他dried

実験手順

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.

出典