HRID132722

反应详情

EQUATION

反应方程式

HRID 132722 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

In N2 atmosphere free of water and oxygen, to a 3-neck flask placed in an ice-bath and equipped with addition funnel and reflux condenser were successively added 0.07 mol sodium hydride and 100 ml tetrahydrofuran. To the mixture was added dropwise a solution of 0.06 mol ethyl butyrate and 0.03 mol butanone with stirring. Upon completing the addition, the mixture was heated refluxing for 4 hours. The solvent and composition with a boiling point below 110° C. were removed by distillation. To the residue was added an appropriate amount of saturated saline until the solid composition was just dissolved. The mixture was extracted with ethyl ether for three times. The organic phases were combined and dried over anhydrous sodium sulfate. The solvent was removed by distillation to give 2.4 g product.

WORKUP

后处理

  1. customequipped with addition funnel
  2. temperaturereflux condenser
  3. additionthe addition
  4. temperaturethe mixture was heated
  5. temperaturerefluxing for 4 hours
  6. customThe solvent and composition with a boiling point below 110° C. were removed by distillation
  7. additionTo the residue was added an appropriate amount of saturated saline until the solid composition
  8. dissolutionwas just dissolved
  9. extractionThe mixture was extracted with ethyl ether for three times
  10. dry with materialdried over anhydrous sodium sulfate
  11. customThe solvent was removed by distillation