反应详情

温度

140 °C

Sodium hydroxide (10 g, 0.25 mol) and hydrazine monohydrate (10 mL) were added to a solution of 3-acetyl-5-bromopyridine (5 g, 25 mmol) dissolved in diethylene glycol (18 mL). The reaction mixture was heated to 140° C. for 6 hours and then partitioned between H2O and Ether. The organic layers were washed with brine, dried over MgSO4 and concentrated. The residue was purified by flash silica gel chromatography (0% to 40% EtOAc in hexanes) to give the title compound (3 g, 65%). 1H NMR (400 MHz, CDCl3): δ 1.26 (t, J=7.6 Hz, 3 H), 2.65 (q, J=7.6 Hz, 2 H), 7.67 (s, 1 H), 8.37 (s, 1 H), 8.51 (s, 1 H).

1. custompartitioned between H2O and Ether
2. washThe organic layers were washed with brine
3. dry with materialdried over MgSO4
4. concentrationconcentrated
5. customThe residue was purified by flash silica gel chromatography (0% to 40% EtOAc in hexanes)