反应详情

温度

7.5 °C

To a suspension of 3-amino-5-(tert-butyl)selenophene-2-carbonitrile (5.0 g) in aqueous sodium hydroxide solution (80 mL, 10%) was added ethanol (50 mL) and the mixture refluxed for 1 h. Ethanol was distilled off under vacuum (appr. 25 mL) and the mixture was allowed to cool to 5-10° C. The separated crystals were filtered off, washed with cold water and dried to give the product as a off-white color solid (4.5 g, 84%), mp 160-162° C. 1H NMR (400 MHz, CDCl3): δ 6.58 (1H, s, H-4), 5.75 (2H, br s, —CONH2), 5.13 (2H, br s, —NH2), 1.34 (9H, s, tert-butyl).

1. temperaturethe mixture refluxed for 1 h
2. distillationEthanol was distilled off under vacuum (appr. 25 mL)
3. filtrationThe separated crystals were filtered off
4. washwashed with cold water
5. customdried