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
To a suspension of N-(4-((piperazin-1-yl)methyl)-phenylmethyl)acetamide (1.0 g) obtained in Example 78(2) and 2,4-dichloropyrimidine (0.60 g) in acetonitrile (20 ml) was added potassium carbonate (0.84 9) and the mixture was stirred at room temperature for 2 hr. The reaction mixture was poured into water (200 ml) and extracted with ethyl acetate (100 ml). The extract was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated and the obtained residue was purified by silica gel column chromatography (developing solvent; ethyl acetate:methanol=20:1-10:1) to give N-(4-((4-(2-chloropyrimidin-4-yl)piperazin-1-yl)methyl)phenylmethyl)acetamide (0.61 g) as white crystals and N-(4-((4-(4-chloropyrimidin-2-yl)piperazin-1-yl)methyl)phenylmethyl)acetamide (10 mg) as white crystals. N-(4-((4-(2-chloropyrimidin-4-yl)piperazin-1-yl)methyl)phenylmethyl)acetamide.
WORKUP
后处理
- extractionextracted with ethyl acetate (100 ml)
- washThe extract was washed with saturated brine
- dry with materialdried over anhydrous magnesium sulfate
- customThe solvent was evaporated
- customthe obtained residue was purified by silica gel column chromatography (developing solvent; ethyl acetate:methanol=20:1-10:1)