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 prepared by dissolving 3.59 g (10.66 mM) of 3-carbethoxy-5-chloromethylimidazo[1,2-a]pyridine sulfate, 3.10 g (12.79 mM) of 3-(1-tert-butoxycarbonylpiperidin-4-yl)-1-propylamine, and 5.94 ml (42.64 mM) of triethylamine in 30 ml of ethanol was refluxed for 5 hours. After completion of the reaction, the solvent was distilled off under reduced pressure and the residue was extracted with 100 ml of chloroform. The organic layer was washed with 100 ml of saturated aqueous NaCl solution and dried over MgSO4 and the solvent was distilled off under reduced pressure. The residue was purified by silica gel column chromatography (eluent: chloroform-methanol=50:1) to provide 2.55 g (yield 62.1%) of the title compound as yellow oil.
WORKUP
后处理
- customA solution prepared
- temperaturewas refluxed for 5 hours
- customAfter completion of the reaction
- distillationthe solvent was distilled off under reduced pressure
- extractionthe residue was extracted with 100 ml of chloroform
- washThe organic layer was washed with 100 ml of saturated aqueous NaCl solution
- dry with materialdried over MgSO4
- distillationthe solvent was distilled off under reduced pressure
- customThe residue was purified by silica gel column chromatography (eluent: chloroform-methanol=50:1)