反应详情

温度

7.5 °C

To a suspension of 3-aminoselenopheno[2,3-b]pyridine-2-carbonitrile (1.0 g) in aqueous sodium hydroxide solution (20 mL, 10%) was added ethanol (20 mL) and the mixture refluxed for 45 min. Ethanol was distilled off under vacuum (appr. 25 mL) and the mixture was allowed to cool to 5-10° C. The separated crystals and the solution was poured into ice cooled water and stirred for 15 min. The solid was filtered off, washed with cold water and dried to give the product as a pale yellow color solid (0.53 g, 50%), mp 256-260° C. 1H NMR (400 MHz, DMSO-d6): δ 8.60 (1H, d, J=3.6 Hz, H-6), 8.37 (1H, d, J=7.6 Hz, H-4), 7.47 (1H, dd, J=8.0, 4.8 Hz, H-5), 7.32 (2H, s, —CONH2), 7.09 (2H, s, —NH2); LC-MS (negative ion mode): m/z 238, 241 (M−H)−.

1. temperaturethe mixture refluxed for 45 min
2. distillationEthanol was distilled off under vacuum (appr. 25 mL)
3. additionThe separated crystals and the solution was poured into ice
4. temperaturecooled water
5. filtrationThe solid was filtered off
6. washwashed with cold water
7. customdried