HRID326125

反应详情

EQUATION

反应方程式

HRID 326125 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureat reflux temperature for 30 minutes under an atmosphere of nitrogen
  2. customThe xylene is then removed by distillation under reduced pressure
  3. dissolutionthe residue is dissolved in 15 ml of diethyl ether
  4. custompurified by column chromatography on silica gel
  5. washThe product is eluted
  6. additiona 2:1 mixture of diethyl ether and ethyl acetate as eluent
  7. customEvaporation of the solvent