反应详情

温度

70 °C

2,6-dichloropyridine-4-carbonitrile 24 (4 gr, 23.13 mmol) was dissolved in 100 ml of ethanol. To the solution were added TEA (1 equiv., 3.22 ml), morpholine (1 equiv., 2 ml) and the mixture was stirred at 70° C. for 4 hours. (TLC AcOEt 3/petroleum ether 7). The solvent was evaporated and the residue was dissolved with ethyl acetate, washed with water and brine. The organic phase was dried over sodium sulfate and concentrated under vacuum. The crude was crystallized from ethyl acetate and petroleum ether to give a beige solid. (4.6 g, 89% yield) 1HNMR (DMSO, 400 MHz) δ 3.58 (4H, m), 3.64 (4H, m), 7.10 (1H, s), 7.32 (1H, s)

1. customThe solvent was evaporated
2. dissolutionthe residue was dissolved with ethyl acetate
3. washwashed with water and brine
4. dry with materialThe organic phase was dried over sodium sulfate
5. concentrationconcentrated under vacuum
6. customThe crude was crystallized from ethyl acetate and petroleum ether
7. customto give a beige solid