反应详情

温度

80 °C

A mixture of crude 2-bromo-1-(4-iodophenyl)ethanone (18.2 g), 2-amino-3-picoline (1.1 equiv, 61.6 mmol), and sodium bicarbonate (1.3 equiv, 72.8 mmol) in isopropanol (160 mL) was heated at 80° C. for 16 h. After concentrating the reaction mixture in vacuo, water (100 mL) was added and the resultant tan slurry was filtered, rinsing with water (2×50 mL). The brown solid was recrystallized from hot isopropanol and further dried in vacuo to provide the title product as a brown solid (13.2 g, 71%). ESMS [M+H]+: 335.0.

1. concentrationAfter concentrating the reaction mixture in vacuo, water (100 mL)
2. additionwas added
3. filtrationthe resultant tan slurry was filtered
4. washrinsing with water (2×50 mL)
5. customThe brown solid was recrystallized from hot isopropanol
6. customfurther dried in vacuo