反应详情

To a 50° C. solution of 0.158 g of 7-amino-4-(3-bromoanilino)-quinazoline (J Med Chem, 1995:3482) in 10 mL of tetrahydrofuran was added 0.059 g of maleic anhydride. The cold solution stirred for 15 minutes, and then the ice bath was removed. The reaction warmed to room temperature where it continued stirring for 15 hours. The suspension was heated under reflux for 30 minutes and then stirred at room temperature another 15 hours. Another 0.059 g of maleic anhydride and 20 mL of tetrahydrofuran were added, and the reaction was refluxed for an additional 2 hours. After another 15 hours at room temperature, the reaction was refluxed for 15 hours. The reaction was filtered, and the light tan solid was recrystallized first from dimethyl-formamide and then a second time from methanol to afford 0.036 g of the desired product.

1. customthe ice bath was removed
2. stirringcontinued stirring for 15 hours
3. temperatureThe suspension was heated
4. temperatureunder reflux for 30 minutes
5. stirringstirred at room temperature another 15 hours
6. additionAnother 0.059 g of maleic anhydride and 20 mL of tetrahydrofuran were added
7. temperaturethe reaction was refluxed for an additional 2 hours
8. waitAfter another 15 hours at room temperature
9. temperaturethe reaction was refluxed for 15 hours
10. filtrationThe reaction was filtered
11. customthe light tan solid was recrystallized first from dimethyl-formamide