HRID1162355
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-benzylpiperazine (6.8 g) and 4-chloro-2-methylpyridine (4.9 g) in acetic acid (20 ml) was heated under reflux for 15 hours, and then concentrated under reduced pressure. The residue was dissolved in water, and the reaction mixture was basified with potassium carbonate and extracted with ethyl acetate. The extract was dried over anhydrous magnesium sulfate, and the solvent was distilled off under reduced pressure. The residue was purified with basic silica gel column (ethyl acetate) to obtain the title compound as a brown oil (10 g, quantitative).
WORKUP
后处理
- temperatureunder reflux for 15 hours
- concentrationconcentrated under reduced pressure
- dissolutionThe residue was dissolved in water
- extractionextracted with ethyl acetate
- dry with materialThe extract was dried over anhydrous magnesium sulfate
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was purified with basic silica gel column (ethyl acetate)