反应详情

温度

5 °C

To an ice cold solution of 0.158 g of 7-amino-4(3-bromoanilino)-quinazoline and 0.216 g of monoethyl fumarate in 3 mL of dry dimethylformamide was added 0.288 g of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide HCl (EDAC). 7-Amino-4-(3-bromoanilino)quinazoline can be made by methods well-known to those skilled in the art. See, for example, J Med Chem, 1995:3482, which is hereby incorporated by reference. After stirring at 5° C. for 5 minutes, the ice bath was removed, and the reaction was permitted to warm to room temperature where it stirred for 15 hours. The reaction was poured into cold water, and the suspension was made basic with the addition of a saturated sodium bicarbonate solution. The resulting solid was collected by filtration, washed with water, and then recrystallized from 50 mL of ethanol to afford 0.052 g of the desired product, mp >260° C.

1. customthe ice bath was removed
2. temperatureto warm to room temperature where it
3. stirringstirred for 15 hours
4. additionThe reaction was poured into cold water
5. additionthe suspension was made basic with the addition of a saturated sodium bicarbonate solution
6. filtrationThe resulting solid was collected by filtration
7. washwashed with water
8. customrecrystallized from 50 mL of ethanol