反应详情

温度

40 °C

2M Aqueous sodium hydroxide (0.3 ml, 6 mmol) was added to a solution of 4-(2-fluoro-5-methoxycarbonyloxy-4-methylanilino)-7-(2-(imidazol-1-yl)ethoxy)-6-methoxyquinazoline (257 mg, 5.5 mmol) in methanol (5 ml) and the mixture stirred for 1 hour at 40° C. Water and 1M hydrochloric acid (0.6 ml) were added and the mixture concentrated to half volume by evaporation. The resulting solid was collected by filtration, dissolved in methylene chloride/methanol and a solution of 7M hydrogen chloride in isopropanol (0.4 ml) was added. The volatiles were removed by evaporation, the solid residue was triturated with ether, collected by filtration and dried under vacuum to give 4-(2-fluoro-5-hydroxy-4-methylanilino)-7-(2-(imidazol-1-yl)ethoxy)-6-methoxyquinazoline hydrochloride (160 mg, 60%).

1. concentrationthe mixture concentrated to half volume by evaporation
2. filtrationThe resulting solid was collected by filtration
3. dissolutiondissolved in methylene chloride/methanol
4. additiona solution of 7M hydrogen chloride in isopropanol (0.4 ml) was added
5. customThe volatiles were removed by evaporation
6. customthe solid residue was triturated with ether
7. filtrationcollected by filtration
8. customdried under vacuum