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硫酸氢钠催化合成季戊四醇双缩醛(酮)

     

摘要

Pentaerythritol diacetals or diketals were synthesized with catalysis of sodium hydrogen sulfate u-sing pentaerythritol,aldehyde or ketone as materials. The influence of the molar ratio of reactants, the type of catalyst and its dosage,the type of water-carrying agent and its dosage on the yield were investigated. For pentaerythritol dicyclohexanone,the optimal reaction conditions were obtained as follows:the molar ratio of pentaerythritol and cyclohexanone was 1 : 2. 2,the catalyst was sodium hydrogen sulfate of 0. 8 g,and the water-carrying agent was toluene of 30 mL. The yields of products were more than 83%. Besides,the products were characterized by IR,elemental analysis,1 HNMR and melting point.%以季戊四醇和醛(酮)为原料、硫酸氢钠为催化剂,合成了季戊四醇双缩醛(酮)化合物.探索了物料配比[n(季戊四醇)∶n(醛/酮),下同]、催化剂种类及用量、带水剂种类及用量等反应条件对产率的影响.以季戊四醇双缩环己酮为例,确定其适宜合成条件如下:物料配比为1∶2.2,催化剂硫酸氢钠用量为0.4g,带水剂甲苯用量为30 mL.制得的季戊四醇双缩醛(酮)产率在83%以上.通过红外光谱、元素分析、1HNMR和熔点对产品进行了物性和结构表征.

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