反应详情

温度

110 °C

A solution of 6-methylpyridine-2,4-diol (1.75 g, 14.0 mmol) in dry DMF (6.0 mL) is stirred under N2 and phosphorus oxybromide (3.05 g, 10.6 mmol) is added in one portion. The mixture is heated at 110° C. for 45 min and then cooled and diluted with water (7 mL). Na2CO3 (s) is added to bring the pH to 7 and the resulting suspension is cooled to 0° C. The product is collected by suction filtration, rinsing with cold water and diethyl ether, and dried overnight in a vacuum desiccator to afford the title compound as a light brown solid (920 mg).

1. temperaturecooled
2. temperaturethe resulting suspension is cooled to 0° C
3. filtrationThe product is collected by suction filtration
4. washrinsing with cold water and diethyl ether
5. customdried overnight in a vacuum desiccator