反应详情

To a solution of 3-(3-nitropyridin-4-yl)-2-oxopropionic acid ethyl ester (Preparation 13, 500 mg, 2.1 mmol) in ethanol (20 mL) and THF (10 mL) was added saturated ammonium chloride solution (10 mL) and iron powder (700 mg, 12.6 mmol). The reaction was heated under reflux for 1 h, then filtered through celite and washed through with hot ethyl acetate (3×30 mL). The combined organic fractions were washed with brine (20 mL), dried (MgSO4) and concentrated in vacuo to give the title compound as a brown solid. δH (CD3OD): 1.44 (3H, t), 4.43 (2H, q), 7.21 (1H, s), 7.69 (1H, d), 8.12 (1H, d), 8.80 (1H, s).

1. temperatureThe reaction was heated
2. temperatureunder reflux for 1 h
3. filtrationfiltered through celite
4. washwashed through with hot ethyl acetate (3×30 mL)
5. washThe combined organic fractions were washed with brine (20 mL)
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo