반응 #53292

반응 방정식

HCl

Ethyl 4-(4-(2,5-Difluorobenzyloxy)phenyl)-4-oxobutyrate

Ethyl 4-(4-(2,5-difluorobenzyloxy)phenyl)-4-oxobutyrate

NaOH

→

title compound

4-(4-(2,5-Difluorobenzyloxy)phenyl)-4-oxobutyric acid

용매

ethanol

반응 조건

후처리

1. 1
   농축concentrated in vacuo
2. 2
   세척washed with water
3. 3
   세척The aqueous layer was washed one more time with chloroform
4. 4
   건조The combined organic layers were dried over Na2SO4
5. 5
   여과filtered
6. 6
   농축concentrated
7. 7
   기타The purification

실험 절차

To a solution of Ethyl 4-(4-(2,5-Difluorobenzyloxy)phenyl)-4-oxobutyrate (Step B, 16.51 g, 47.4 mmol) in abs ethanol (100 ml) was added 1N NaOH (40 ml) at room temperature. The reaction mixture was stirred for 3 hours, acidified with 1M HCl and concentrated in vacuo. The crude mixture was taken in chloroform and washed with water. The aqueous layer was washed one more time with chloroform. The combined organic layers were dried over Na2SO4, filtered and concentrated. The purification was done by flash. chromatography on silica gel column (chloroform:methanol, 95:5 spiked with acetic acid) to provide the title compound as a white solid.

출처