反应详情

温度

100 °C

A mixture of 7-hydroxy-6-methoxyquinazolin-4-(3H)-one (8.0 g, 41.6 mmol), pyridine (7.5 ml) and acetic anhydride (63 ml) was heated at 100° C. for 4.5 hours and left to cool to ambient temperature 18 hours. The reaction mixture was poured into ice/water (400 ml) and the resultant precipitate collected by filtration and dried in vacuo. Analysis revealed that hydrolysis of the acetate group on the 4 position of the quinazoline was incomplete. The mixture was therefore treated with water (150 ml) and pyridine (0.5 ml) at 90° C. for 15 minutes. The reaction was cooled and the solid was collected by filtration, washed with water and dried in vacuo to yield 7-(acetoxy)-6-methoxyquinazolin-4-(3H)-one (7.4 g, 76% yield):

1. waitleft
2. temperatureto cool to ambient temperature 18 hours
3. filtrationthe resultant precipitate collected by filtration
4. customdried in vacuo
5. customAnalysis revealed that hydrolysis of the acetate group on the 4 position of the quinazoline
6. temperatureThe reaction was cooled
7. filtrationthe solid was collected by filtration
8. washwashed with water
9. customdried in vacuo