반응 #1106642

반응 방정식

NaOH

1-(2-hydroxy-4-(methoxymethoxy)phenyl)-3-(6-methoxypyridin-3-yl)propan-1-one

TFA

→

white solid

수율 35.8%

2,4-dihydroxyphenyl-3-(6-methoxypyridin-3-yl)propan-1-one

수율 35.8%

용매

CH3CN

반응 조건

후처리

1. 1
   추출The aqueous was extracted with 100 ml EtOAc
2. 2
   세척The organic layer was washed with brine
3. 3
   건조dried (Na2SO4)
4. 4
   농축concentrated
5. 5
   기타The residue was purified by silica gel chromatography (15% EtOAc/Hexane)

실험 절차

To a solution of 1-(2-hydroxy-4-(methoxymethoxy)phenyl)-3-(6-methoxypyridin-3-yl)propan-1-one (1.62 g, 5.11 mmol) in CH3CN (30 ml) at room temperature was added TFA (2 ml) dropwise, two drops of water. The reaction was stirred at same temperature for 8 h. Aqueous 1N NaOH was added to the reaction mixture until pH=7. The aqueous was extracted with 100 ml EtOAc, and the organic layers were combined. The organic layer was washed with brine, dried (Na2SO4) and concentrated. The residue was purified by silica gel chromatography (15% EtOAc/Hexane) to provide 0.5 g (35%) of white solid.

출처