1,2-二苯氧基乙烷的合成及工艺

Synthesis of 1,2-diphenoxyethane and optimized process

摘要:

采用水相体系直接合成得到高纯度的1,2-二苯氧基乙烷，在优化的工艺条件下，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/批扩大合成试验评价，效果稳定。最优合成工艺为：反应时间25h，w(KOH)=50%，n(KOH):n(苯酚):n(1,2-二溴乙烷)=3.0:3.0:1.0，反应温度为60℃。在上述条件下，产物中杂质的生成量较少。

Abstract:

1,2-diphenoxyethane with high purity was successfully synthesized by reacting 1,2-dibromoethane 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, and this attractive result was confirmed by a series of scale-up test with 10kg/batch size. The following optimized con-ditions were obtained: the optimized reaction time is 25h, 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 opti-mized conditions, the impurity contained in the final product can be decreased to a limited level.