HRID478731

反应详情

EQUATION

反应方程式

HRID 478731 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of diethyl malonate (9.6 g, 0.06mol) in 20 ml of absolute ethanol was added sodium ethoxide (4.1 g) portionwise at room temperature while stirring and the mixture was further stirred for 4 hours followed by dropwise addition of 4-vinylpyridine (2.1 g, 0.02 mol). The mixture was then stirred overnight. Evaporation of ethanol under reduced pressure gave a residue to which was added water followed by neutralization with 3N hydrochloric acid. The mixture was extracted with ethyl acetate. The extracted liquid was treated according to conventional techniques. Evaporation of solvent yielded a residue which was subjected to purification using column chromatography on silica gel to afford diethyl 2-(pyridin-4-yl)ethylmalonate as an oil (2.46 g, 46%).

WORKUP

后处理

  1. stirringthe mixture was further stirred for 4 hours
  2. stirringThe mixture was then stirred overnight
  3. customEvaporation of ethanol under reduced pressure
  4. customgave a residue to which
  5. extractionThe mixture was extracted with ethyl acetate
  6. additionThe extracted liquid was treated
  7. customEvaporation of solvent
  8. customyielded a residue which
  9. customwas subjected to purification