Reaktion #1106642

Reaktionsgleichung

NaOH

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

TFA

→

white solid

Ausbeute 35.8%

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

Ausbeute 35.8%

Lösungsmittel

CH3CN

Reaktionsbedingungen

Aufarbeitung

1. 1
   ExtraktionThe aqueous was extracted with 100 ml EtOAc
2. 2
   WaschenThe organic layer was washed with brine
3. 3
   Trocknendried (Na2SO4)
4. 4
   Einengenconcentrated
5. 5
   SonstigeThe residue was purified by silica gel chromatography (15% EtOAc/Hexane)

Vorschrift

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.

Quelle