反应详情

温度

55 °C

To 10 mL of H2SO4 (97%) kept in an ice-bath was added portionwise 2.45 g (16.6 mmol) of 2-amino-4,6-dimethyl-5-pyridinecarbonitrile (16) and it was stirred for 30 min. The resulting solution was heated at 55° C. and 1.2 mL (18.8 mmol) of HNO3 (d=1.41, 69-70%) was added dropwise. The solution was heated at 55°-60° C. for 3 h after addition of HNO3. It was cooled to room temperature and poured into 60 mL of ice-water. The yellow precipitate was filtered, washed with water, and dried to leave a yellow solid (1.76 g, 55%). 1H NMR (CDCl3), 2.612 (s, 3), 2.716 (s, 3), 6.51 (mb, 2).

1. temperatureThe solution was heated at 55°-60° C. for 3 h
2. temperatureIt was cooled to room temperature
3. filtrationThe yellow precipitate was filtered
4. washwashed with water
5. customdried