HRID970414
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 1.2 g (5.3 mmol) of 5-bromo-2,4-dichloro-pyrimidine in 30 ml of acetonitrile is added to a solution of 1.5 g (5.2 mmol) of N-(5-amino-pentyl)-3-nitro-benzenesulfonamide in 50 ml of acetonitrile. The reaction mixture is mixed with 1.0 ml (7.2 mmol) of triethylamine and stirred for 17 hours at room temperature. After water (50 ml) is added, it is extracted (2×) with ethyl acetate. The combined organic phases are dried (Na2SO4), filtered and concentrated by evaporation. The remaining residue is purified by chromatography (hexane/ethyl acetate 2:1, Flashmaster II). 1.5 g (3.1 mmol, corresponding to 60% of theory) of the product is obtained.
WORKUP
后处理
- extractionit is extracted (2×) with ethyl acetate
- dry with materialThe combined organic phases are dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated by evaporation
- customThe remaining residue is purified by chromatography (hexane/ethyl acetate 2:1, Flashmaster II)
- custom1.5 g (3.1 mmol, corresponding to 60% of theory) of the product is obtained