β-Bromoalkenyl sulfide is synthesized from diphenylacetylene and p-toluene disulfide under the mixed hydrobromic acid-nitric acid catalytic system.A non-destructive and rapid method for the analysis of β-bromoalkenyl sulfide content in the reaction system is established by means of Raman spectroscopy and space angle conversion methods.The effects of mixed acids ratio,raw materials ratio and reaction temperature on the yield of β-bromoalkenyl sulfide are investigated through designing response surface optimization experiments.Study results show that the optimum conditions for the synthesis of β-bromoalkenyl sulfide are as follows;The molar ratio of hydrobromic acid to nitric acid is 10∶0.5,the molar ratio of diphenylacetylene to p-toluene disulfides is 2∶1,reaction temperature is 40℃,and reaction time is 4 h.Under these conditions,the yield ofβ-bromoalkenyl sulfide reaches 90.52%.