4-苯硫基苯酚的合成及表征

以苯硫酚钠和对硝基氯苯为原料,经过取代、还原、重氮化、水解4步反应,最终合成了4-苯硫基苯酚,通过单因素实验确定了还原反应的较佳条件是:原料配比n(4-硝基二苯硫醚):n(水合肼)=1:2.5,催化剂三氯化铁用量为4-硝基二苯硫醚质量的3.0%,反应温度70℃,反应时间4.5h。目标产物4-苯硫基苯酚总收率约为64%,纯度为95%。目标产物的结构通过IR、GC-MS和1 H NMR进行了确证。

Preparation and Characterization of 4-Thiophenylphenol

4-Thiophenylphenol was synthesized using sodium thiophenoxide and 4-nitrochlorobenzene as raw materials by nucleophilic substitution,reduction,diazotization,and hydrolysis.The reduction conditions were optimized and the obtained optimum conditions were n(4-nitrodiphenyl sulfide):n(hydrazine hydrate)=1:2.5,catalyst dosage 3%(based on the weight of 4-nitrodiphenyl sulfide),reaction temperature 70 ℃ and time 4.5 h.The yield of 4-thiophenylphenol was about 64% with the purity of 95%.The structure of the target compound was determined by IR,MS and 1H NMR.