HRID346544
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-bromo-2-fluoroanilino)-6-methoxyquinazoline hydrochloride (9.4 g, 19.1 mmol) in TFA (90 ml) was heated at reflux for 50 minutes. The mixture was allowed to cool and was poured on to ice. The resulting precipitate was collected by filtration and dissolved in methanol (70 ml). The solution was adjusted to pH 9–10 with concentrated aqueous ammonia solution. The mixture was concentrated to half initial volume by evaporation. The resulting precipitate was collected by filtration, washed with water and then ether, and dried under vacuum to give 4-(4-bromo-2-fluoroanilino)-7-hydroxy-6-methoxyquinazoline (5.66 g, 82%).
WORKUP
后处理
- temperatureat reflux for 50 minutes
- temperatureto cool
- additionwas poured on to ice
- filtrationThe resulting precipitate was collected by filtration
- dissolutiondissolved in methanol (70 ml)
- concentrationThe mixture was concentrated to half initial volume
- customby evaporation
- filtrationThe resulting precipitate was collected by filtration
- washwashed with water
- dry with materialether, and dried under vacuum