反应详情

温度

190 °C

A mixture of 3-(4-bromophenoxy)-picolinonitrile (57 g, 207 mmol) and 300 g of PPA was stirred at 190° C. for 2 h, followed by 180° C. overnight. After cooling to RT, the reaction mixture was poured into 500 g of ice water. After the PH was adjusted to 7 with KOH, the suspension was filtered. The solid was washed with large excess of water, followed by washing with methanol and acetone. The resulting solid was air dried to give 8-bromo-10H-chromeno[3,2-b]pyridin-10-one as a tan solid with >90% purity. The material was carried on to the next step.

1. waitfollowed by 180° C. overnight
2. temperatureAfter cooling to RT
3. filtrationthe suspension was filtered
4. washThe solid was washed with large excess of water
5. washby washing with methanol and acetone
6. customdried