反应详情

温度

0 °C

To an ice cold solution (0° C.) of 3-amino-5-(tert-butyl)selenophene-2-carboxamide (3.0 g, 12.2 mmol) in concentrated sulfuric acid (50 mL) was added a cold (0° C.) solution of sodium nitrite (0.92 g, 13.4 mmol) in concentrated sulfuric acid (10 mL) for 10 min (while adding, the temperature should keep between −5-0° C.). After addition, the mixture was stirred at 0° C. for 1 h and at rt for 1 h. The reaction mixture was cooled and poured into crushed ice slowly with stirring for 15 min and stirred at the same temperature for 15 min. The solid was filtered, washed with ice cold water and dried to give the product as a off-white color solid (2.4 g, 77%), mp 158-160° C. 1H NMR (400 MHz, CDCl3): δ 7.67 (1H, s, H-7), 1.50 (9H, s, tert-butyl); LC-MS (negative ion mode): m/z 254, 256 (M−H)—.

1. additionwhile adding
2. customshould keep between −5-0° C.
3. additionAfter addition
4. temperatureThe reaction mixture was cooled
5. additionpoured
6. custominto crushed ice slowly
7. stirringwith stirring for 15 min
8. stirringstirred at the same temperature for 15 min
9. filtrationThe solid was filtered
10. washwashed with ice cold water
11. customdried