反应详情

温度

120 °C

12.0 g (42.84 mmol) of 7-(2,4-dichlorophenyl)imidazo[1,2-c]pyrimidin-5-ol are introduced into 131.6 g (858.27 mmol) of phosphoryl chloride and heated at 120° C. for 5 h. A clear solution is produced after 10 min. The mixture is allowed to cool, and then 2000 ml of saturated aqueous sodium bicarbonate solution are cautiously added. Towards the end, about 100 g of solid sodium bicarbonate are also added, and the mixture is stirred at pH 7 for 10 min. The precipitate is filtered off with suction, thoroughly washed with water, suspended in a little isopropanol and sucked dry. It is then washed once more with petroleum ether and dried under high vacuum at 50° C. 11 g (81% of theory) of the product are obtained as a solid.

1. customA clear solution is produced after 10 min
2. temperatureto cool
3. filtrationThe precipitate is filtered off with suction
4. washthoroughly washed with water
5. customsucked dry
6. washIt is then washed once more with petroleum ether
7. customdried under high vacuum at 50° C
8. custom11 g (81% of theory) of the product are obtained as a solid