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