HRID1168691
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
2.77 ml of triethylamine, 3.43 g of diethoxyphosphorylacetic acid, and 5.62 g of benzotriazol-1-yl-N-tetramethyluronium tetrafluoroborate are added successively to 5.00 g of 6-amino-4-[(3-chloro-4-fluorophenyl)amino]-7-cyclopropylmethoxyquinazoline in 25 ml of N,N-dimethylformamide. The reaction mixture is stirred for one hour at ambient temperature; 250 ml of water is then added and the mixture is extracted with 250 ml of ethyl acetate/methanol (10:1). The organic phase is washed with water and saturated sodium chloride solution, dried over magnesium sulfate, and concentrated by evaporation. The residue in the flask is crystallized by stirring with diethylether.
WORKUP
后处理
- extractionthe mixture is extracted with 250 ml of ethyl acetate/methanol (10:1)
- washThe organic phase is washed with water and saturated sodium chloride solution
- dry with materialdried over magnesium sulfate
- concentrationconcentrated by evaporation
- customThe residue in the flask is crystallized
- stirringby stirring with diethylether