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
- 80 °C
PROCEDURE
实验过程
2-Oxo-1-[[2-(3,4,5-trimethoxyphenyl)pyridin-4-yl]methyl]piperazine (62 mg) was dissolved in acetonitrile (5 mL), and to the solution potassium carbonate (24 mg), potassium iodide (29 mg) and 4-chloromethyl-2-(3,4,5-trimethoxyphenyl)pyridine (51 mg) were added, and the mixture was stirred at 80° C. for 1 hour. The reaction mixture was concentrated under reduced pressure, ethyl acetate was added to the residue, and the resultant mixture was washed with a saturated aqueous solution of sodium hydrogencarbonate, water and saturated brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure. The resultant oil was purified by preparative TLC on silica gel (chloroform:methanol=25:1) to obtain the title compound as a hydrochloride.
WORKUP
后处理
- concentrationThe reaction mixture was concentrated under reduced pressure, ethyl acetate
- additionwas added to the residue
- washthe resultant mixture was washed with a saturated aqueous solution of sodium hydrogencarbonate, water and saturated brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated under reduced pressure
- customThe resultant oil was purified by preparative TLC on silica gel (chloroform:methanol=25:1)