HRID279546
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 7-benzyloxy-4-(4-chloro-2-fluoroanilino)-6-methoxyquinazoline hydrochloride (892 mg, 2 mmol) in TFA (10 ml) was heated at reflux for 50 minutes. The mixture was allowed to cool and then poured on to ice. The precipitate was collected by filtration, dissolved in methanol (10 ml) and basified to pH11 with aqueous ammonia. The mixture was concentrated by evaporation, the resulting solid product was collected by filtration, washed with water then ether and dried under vacuum to give 4-(4-chloro-2-fluoroanilino)-7-hydroxy-6-methoxyquinazoline (460 mg, 72%) as a yellow solid.
WORKUP
后处理
- temperatureat reflux for 50 minutes
- temperatureto cool
- additionpoured on to ice
- filtrationThe precipitate was collected by filtration
- dissolutiondissolved in methanol (10 ml)
- concentrationThe mixture was concentrated by evaporation
- filtrationthe resulting solid product was collected by filtration
- washwashed with water
- dry with materialether and dried under vacuum