反应详情

A mixture of 12.4 g. of 6-dimethylamino-quinazolin-4(3H)-one and 50 ml. of phosphorus oxychloride is refluxed under nitrogen for 10 minutes, cooled to room temperature, 150 ml. of ether added, the crystals recovered by filtering, washed with ether and dried. The solids are added to 500 ml. of ice-water, concentrated ammonia is added to neutralize the solution which is extracted with 1.0 liter of chloroform. The chloroform extract is dried and filtered through 300 ml. of silica gel using chloroform as an eluant. Evaporation of the eluant yields 6-dimethylamino-4-chloroquinazoline, m.p. 126°-127.5° C.

1. additionA mixture of 12.4 g
2. customthe crystals recovered
3. filtrationby filtering
4. washwashed with ether
5. customdried
6. additionThe solids are added to 500 ml
7. additionof ice-water, concentrated ammonia is added
8. extractionis extracted with 1.0 liter of chloroform
9. extractionThe chloroform extract
10. customis dried
11. filtrationfiltered through 300 ml
12. customEvaporation of the eluant