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
CONDITIONS
反应条件
- 温度
- 45 °C
PROCEDURE
实验过程
A mixture of 4-(4-bromo-2-fluoroanilino)-7-hydroxy-6-methoxyquinazoline (1.2 g, 3.3 mmol), (prepared as described for the starting material in Example 48), 1-bromo-3-chloropropane (1.6 ml, 16 mmol) and potassium carbonate (2.1 g, 15 mmol) in DMF (25 ml) was heated at 45° C. for 3 hours. The mixture was allowed to cool, was diluted with water and extracted with ethyl acetate (3×70 ml). The organic extracts were combined, washed with water and brine, dried (MgSO4) and the volatiles were removed by evaporation. The residue was triturated with hexane/ethyl acetate, collected by filtration and dried under vacuum to give 4-(4-bromo-2-fluoroanilino)-7-(3chloropropoxy)-6-methoxyquinazoline (492 mg; 34%).
WORKUP
后处理
- custom(prepared
- temperatureto cool
- extractionextracted with ethyl acetate (3×70 ml)
- washwashed with water and brine
- dry with materialdried (MgSO4)
- customthe volatiles were removed by evaporation
- customThe residue was triturated with hexane/ethyl acetate
- filtrationcollected by filtration
- customdried under vacuum