反应详情

A 500 ml 3 necked flash fitted with a stirrer, reflux condenser and protected by a calcium chloride trap was charged with 9.0 g of phosphorus pentachloride (0.043 mole) and 70 ml of phosphorus oxychloride and the mixture stirred. To this 11.3 g (0.04 mole) of 2-[2-(5-nitro-2-furyl)vinyl] -4-(3H)quinazolinone was added and rinsed into the flask with 15 ml of phosphorus oxychloride. The mixture was heated under reflux for 4 hours, cooled in an ice bath and diluted with 150 ml of diethyl ether. The 2-[2-(5-nitro-2-furyl)vinyl]-4-chloroquinazoline which precipitated was collected by filtration, washed with 100-150 ml of diethyl ether, slurried in 100 ml of diethyl ether and then refiltered to obtain 8.09 g of the desired product melting at 252°-4°C with decomposition. The product was recrystallized from toluene (large volumes are required) or was extracted in a Soxhlet extractor with toluene to obtain yellow crystals of 2-[2-(5-nitro-2-furyl)vinyl]-4-chloroquinazoline melting at 264°-5°C with decomposition.

1. temperaturereflux condenser
2. customprotected by a calcium chloride trap
3. washrinsed into the flask with 15 ml of phosphorus oxychloride
4. temperatureThe mixture was heated
5. temperatureunder reflux for 4 hours
6. temperaturecooled in an ice bath
7. additiondiluted with 150 ml of diethyl ether
8. customThe 2-[2-(5-nitro-2-furyl)vinyl]-4-chloroquinazoline which precipitated
9. filtrationwas collected by filtration
10. washwashed with 100-150 ml of diethyl ether