HRID326125
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 3 g of 5-[5-ethoxycarbonyl-5-(phenylsulfinyl)pentyl]-imidazo[1,5-a]pyridine in 50 ml xylene is heated at reflux temperature for 30 minutes under an atmosphere of nitrogen. The xylene is then removed by distillation under reduced pressure, the residue is dissolved in 15 ml of diethyl ether and purified by column chromatography on silica gel. The product is eluted using a 2:1 mixture of diethyl ether and ethyl acetate as eluent. Evaporation of the solvent yields 5-(5-ethoxycarbonylpent-4-enyl)-imidazo[1,5-a]pyridine as an oil; NMR (CDC13) 1.29 (t,3H), 4.25 (q,2H), 5.88 (d, 1H).
WORKUP
后处理
- temperatureat reflux temperature for 30 minutes under an atmosphere of nitrogen
- customThe xylene is then removed by distillation under reduced pressure
- dissolutionthe residue is dissolved in 15 ml of diethyl ether
- custompurified by column chromatography on silica gel
- washThe product is eluted
- additiona 2:1 mixture of diethyl ether and ethyl acetate as eluent
- customEvaporation of the solvent