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 5.78 g (24.22 mM) of 3-carbethoxy-5-chloromethylimidazo[1,2-a]pyridine, 7.78 g (36.33 mM) of 1-tert-butoxycarbonyl-4-aminomethylpiperidine, and 6.75 ml (48.44 mM) of triethylamine in 100 ml of ethanol was refluxed under argon gas for 3 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 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=20:1) to provide 6.50 g (yield 72.4%) of the title compound as yellow liquid.
WORKUP
后处理
- customA solution prepared
- temperaturewas refluxed under argon gas for 3 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 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=20:1)