苯基乙烯基砜的制备

为得到一种简单可行的苯基乙烯基砜的合成工艺,文章以苯硫酚、环氧乙烷及浓硫酸为原料进行了研究。实验在间歇釜中针对每个步骤的反应研究了温度、物料比等条件的影响,并探求了较优的反应条件,得到较为理想的反应条件为:苯硫酚与环氧乙烷的反应温度为40℃,二者的摩尔比为1∶1.1,苯硫酚与浓硫酸的摩尔比为1∶3.2,反应温度为140℃。在此条件下的收率为92%。文章还对反应机理进行了讨论。得到的制备苯基乙烯基砜的新工艺过程简捷,操作简单,原子经济性及收率均较高。

Synthesis of phenylvinylsulfone

Thiophenol,ethylene oxide and concentrated sulfuric acid were used as raw materials to prepare phenylvinylsulfone in order to get a simple and applicable synthesis method.The experiments were taken in a batch reactor to investigate the effects of temperature and the ratio of reactants on each step of reactions.The optimum conditions of the reaction were selected as follows: the reaction temperature of thiophenol and ethylene oxide is 40 ℃,the molar ratio of thiophenol to ethylene oxide is 1 ∶1.1,and the reaction temperature of step 2 is 140 ℃,and the molar ratio of thiophenol to concentrated sulfuric acid is 1 ∶3.2.At such conditions the yield is 92%.The new route obtained is much simpler and easier to operate,and has higher atom economy and yield.