反应详情

To a solution of (3-ethoxy-4-nitrophenyl)(2-pyridyl)methanol (2.5 g) in acetic acid (50 ml), reduced iron (7.5 g) was added to the mixture and the mixture was stirred overnight. Ethyl acetate and ethanol were added to the mixture, and the unnecessary substances were filtered off. The filtrate was concentrated under reduced pressure, the residue was diluted with ethyl acetate and neutralized with an aqueous solution of saturated sodium bicarbonate. The organic layer was separated and washed with saturated brine, and dried over magnesium sulfate. The solvent was distilled off under reduced pressure and the obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:2) and recrystallized from hexane-ethyl acetate, to give (4-amino-3-ethoxyphenyl)(2-pyridyl)methanol (340 mg) as crystals.

1. filtrationthe unnecessary substances were filtered off
2. concentrationThe filtrate was concentrated under reduced pressure
3. additionthe residue was diluted with ethyl acetate
4. customThe organic layer was separated
5. washwashed with saturated brine
6. dry with materialdried over magnesium sulfate
7. distillationThe solvent was distilled off under reduced pressure
8. customthe obtained residue was purified by silica gel column chromatography (hexane:ethyl acetate=1:2)
9. customrecrystallized from hexane-ethyl acetate