반응 #42735

반응 방정식

2,3-difluorophenol

aluminium chloride

(4-chlorophenyl)acetyl chloride

→

title compound

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

용매

1,2-dichloroethane

1,2-dichloroethane

water

반응 조건

후처리

1. 1
   온도is heated in an oil bath at 90° C. overnight
2. 2
   온도The reaction mixture is cooled to room temperature
3. 3
   추출extracted with ethyl acetate
4. 4
   건조The organic phase is dried over anhydrous magnesium sulfate
5. 5
   여과filtered
6. 6
   기타evaporated to dryness in vacuo
7. 7
   기타to afford a brown solid
8. 8
   기타This is triturated with hexane/ethyl acetate (9:1)
9. 9
   여과filtered
10. 10
    기타dried

실험 절차

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.

출처