반응 #42737

반응 방정식

Sodium hydride

isobutyric acid 6-[2-(4-chlorophenyl)acetyl]-2,3-difluorophenyl ester

→

title compound

2-(4-Chlorophenyl)-1-(3,4-difluoro-2-hydroxy-phenyl)-4-methyl-pentane-1,3-dione

용매

HCl

tetrahydrofuran

반응 조건

후처리

1. 1
   온도The reaction is cooled to room temperature
2. 2
   세척washed with ethyl acetate
3. 3
   건조The organic phase is dried over anhydrous magnesium sulfate
4. 4
   여과filtered
5. 5
   농축concentrated in vacuo

실험 절차

Sodium hydride (1.5 g, 37.5 mmol, 60% dispersion in mineral oil, 4 eq.) is added portionwise to a stirred solution of isobutyric acid 6-[2-(4-chlorophenyl)acetyl]-2,3-difluorophenyl ester (3.16 g, 8.97 mmol) in tetrahydrofuran (60 ml) over 15 min. The mixture is heated in an oil bath at 80° C. for 4 h. The reaction is cooled to room temperature, diluted with 2M HCl solution and washed with ethyl acetate. The organic phase is dried over anhydrous magnesium sulfate, filtered, and concentrated in vacuo to afford the title compound as a brown oil. The product is used in the next step without further purification.

출처