反应详情

Ammonium chloride (1.1 g, 0.020 mol) dissolved in water (15 mL) was added to a stirred solution of 5-nitro-2-phenyl-pyridine (0.5 g, 2.5 mmol) in THF (10 mL) Methanol (5 mL) was then added, affording a clear solution. Zinc powder (1.3 g, 0.020 mol) was then added portion wise at room temperature and the resulting mixture maintained for 1 hour, then filtered over celite. The filtrate was concentrated and the residue was extracted with ethyl acetate. The organics were washed with brine solution, dried over Na2SO4 and concentrated under reduced pressure to afford 0.35 g (82%) of 6-phenyl-pyridin-3-ylamine. LCMS purity: 171.08 (M+1)+, 87.9%, 1H NMR (DMSO-d6): δ 8.12 (d, 1H), 8.0 (d, 2H), 7.72 (d, 1H), 7.48 (t, 2H), 7.36 (t, 1H), 7.1 (dd, 1H), 5.6 (s, 2).

1. additionwas then added
2. customaffording a clear solution
3. temperaturethe resulting mixture maintained for 1 hour
4. filtrationfiltered over celite
5. concentrationThe filtrate was concentrated
6. extractionthe residue was extracted with ethyl acetate
7. washThe organics were washed with brine solution
8. dry with materialdried over Na2SO4
9. concentrationconcentrated under reduced pressure