反应详情

2M Aqueous sodium hydroxide (1.5 ml, 3 mmol) was added to a solution of 4-(4-chloro-2-fluoro-5-methoxycarbonyloxyanilino)-6-methoxy-7-(3 -(4-pyridyl)propoxy)quinazoline (1.28 g, 2.5 mmol) in methanol (13 ml) and the mixture stirred for 2 hours at ambient temperature. Water was added and the mixture was adjusted to pH7 with 2M hydrochloric acid. The resulting precipitate was collected by filtration, washed with water and dried under vacuum. This solid was dissolved in methylene chloride (30 ml) and methanol (5 ml) and a solution of 5M hydrogen chloride in isopropanol (2.5 ml) was added. The solution was diluted with isopropanol and concentrated under vacuum to a total volume of 10 ml. The resulting solid was collected by filtration, washed with isopropanol and then ether and dried under vacuum to give 4-(4-chloro-2-fluoro-5-hydroxyanilino)-6-methoxy-7-(3-(4-pyridyl)propoxy)quinazoline hydrochloride (924 mg, 70%).

1. filtrationThe resulting precipitate was collected by filtration
2. washwashed with water
3. customdried under vacuum
4. dissolutionThis solid was dissolved in methylene chloride (30 ml)
5. additionmethanol (5 ml) and a solution of 5M hydrogen chloride in isopropanol (2.5 ml) was added
6. additionThe solution was diluted with isopropanol
7. concentrationconcentrated under vacuum to a total volume of 10 ml
8. filtrationThe resulting solid was collected by filtration
9. washwashed with isopropanol
10. dry with materialether and dried under vacuum