1,2-二苯氧基乙烷的合成及工艺

Synthesis of 1,2-Diphenoxyethane and Optimized Process

采用水相体系直接合成得到高纯度的1,2-二苯氧基乙烷,在优化工艺条件下,以1,2-二溴乙烷和苯酚为基本原料,KOH为碱,1,2-二苯氧基乙烷摩尔收率达75%,产品气相色谱纯度达99%,且完成了10 kg/批的扩大合成实验评价,效果稳定。最优合成工艺为:反应时间25 h,w(KOH)=50%的水溶液,n(KOH)∶n(苯酚)∶n(1,2-二溴乙烷)=3.0∶3.0∶1.0,反应温度60℃。在该条件下,产物中杂质的生成量较少。

1,2-Diphenoxyethane with high purity was successfully synthesized by 1,2-dibromoethane reacting with phenol in the aqueous KOH solution.Under the optimized reaction conditions,the molar yield of 1,2-diphenoxyethane exceeding 75% on the basis of 1,2-dibromoethane and GC purity exceeding 99% were achieved.This attractive result was confirmed by a series of scale-up test with 10 kg/batch size.The following optimized conditions were obtained： the optimized reaction time is 25 h,the concentration of base is w（KOH）=50%,and the molar ratio of the main reactants is n（KOH）∶n（phenol）∶n（1,2-dibromoethane）=3.0∶3.0∶1.0.The reaction temperature is 60 ℃.With the above optimized conditions,the impurity contained in the final product can be decreased to a limited level.