反应详情

Add 4-bromo-3-oxo-butyric acid ethyl ester (12.08 g, 57.8 mmol) to a solution of 2-amino-5-bromo pyridine (5.0 g, 28.9 mmol) in acetonitrile (80 mL). Reflux for 4 days and concentrate to dryness. Purify by flash chromatography using appropriate ethyl acetate/methanol mixtures to give the subtitled compound (5.75 g, 70%) as a brown oil. TOF MS ES+ exact mass calculated for C, HI BrN2O2 (p+1): m/z=283.0082 Found: 283.0084. 1H NMR (400 MHz, DMSO-d6) δ 8.68 (m, 1H), 7.82 (s, 1H), 7.45 (d, J=10 Hz, 1H), 7.30 (dd, J=10, 2.0 Hz, 1H), 4.08 (q, J=7.0 Hz, 2H), 3.77 (s, 2H), 1.18 (t, J=7.0 Hz, 3H).

1. temperatureReflux for 4 days
2. concentrationconcentrate to dryness
3. customPurify by flash chromatography