反应详情

A suspension of 4-(2-fluoro-5-methoxycarbonyloxy-4-methylanilino)-6-methoxy-7-(2-(4-pyridyl)ethoxy)quinazoline (300 mg, 0.63 mmol) and 2M aqueous sodium hydroxide (0.38 ml, 0.76 mmol) in methanol (6 ml) was stirred at ambient temperature for 2 hours. Water was added and the mixture adjusted to pH7 with 2M hydrochloric acid. The precipitate was collected by filtration, washed with water, and dried under vacuum. The solid was dissolved in methylene chloride/methanol and a 5M solution of hydrogen chloride in isopropanol (0.5 ml) was added. The mixture was diluted with isopropanol, and the methylene chloride and methanol solvents were removed by evaporation. The resulting precipitate was collected by filtration, washed with methylene chloride and dried under vacuum to give 4-(2-fluoro-5-hydroxy-4-methylanilino)-6-methoxy-7-(2-(4-pyridyl)ethoxy)quinazoline hydrochloride (270 mg, 94%).

1. filtrationThe precipitate was collected by filtration
2. washwashed with water
3. customdried under vacuum
4. dissolutionThe solid was dissolved in methylene chloride/methanol
5. additiona 5M solution of hydrogen chloride in isopropanol (0.5 ml) was added
6. additionThe mixture was diluted with isopropanol
7. customthe methylene chloride and methanol solvents were removed by evaporation
8. filtrationThe resulting precipitate was collected by filtration
9. washwashed with methylene chloride
10. customdried under vacuum