反应详情

温度

-78 °C

Anhydrous ammonia (50 mL) was condensed in a 500 mL 3 necked flasked containing 8-iodo-2,7-dimethyl-4H-benzo[d][1,3]oxazin-4-one (8.5 g, 28 mmol) cooled to −78° C., and the reaction was stirred for 3 h. The cooling bath was removed and the solvent was allowed to evaporate at RT. 1 N Sodium hydroxide (100 mL) was added to the reaction and stirred at reflux for 1 h. The reaction was cooled down to 0° C. and acidified to pH 3 with 5 N HCl. The resulting precipitate was collected by filtration, washed with water and dried in a vacuum oven at 60° C. overnight. 8-Iodo-2,7-dimethylquinazolin-4(3H)-one (8 g, 94% yield) was obtained as a white solid. MS (M+H)+ 301.

1. customThe cooling bath was removed
2. customto evaporate at RT
3. addition1 N Sodium hydroxide (100 mL) was added to the reaction
4. stirringstirred
5. temperatureat reflux for 1 h
6. temperatureThe reaction was cooled down to 0° C.
7. filtrationThe resulting precipitate was collected by filtration
8. washwashed with water
9. customdried in a vacuum oven at 60° C. overnight