PDF全文下载：2011040338
冯柏成， 井丽倩， 刘鹏
（青岛科技大学 化工学院，山东 青岛 266042）
摘要： 以对氯硝基苯作为起始原料，经过取代、还原、重氮化、酯化和碱解-酸化五步反应合成了4,4′-二巯基二苯硫醚，通过单因素实验确定了还原反应的较佳条件：原料配比n（4,4′-二硝基二苯硫醚）∶n（水合肼）=1∶3.03，催化剂三氯化铁用量为4,4′-二硝基二苯硫醚质量的7%，反应温度60～65 ℃，反应时间3 h。目标产物总收率约为50%，纯度为99.5%。目标产物的结构经红外（IR）、气质联用仪（GC-MS）和核磁共振氢谱（1H NMR）进行了确证。
关键词： 4,4′-二巯基二苯硫醚； 还原； 重氮化
中图分类号： O 621.3 文献标志码： A
Preparation and Characterization of 4,4′-Thiodibenzenethiol
FENG Bai-cheng, JING Li-qian, LIU Peng
（College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042,China）
Abstract： 4,4′-Thiodibenzenethiol was prepared using 4-nitrochlorobenzene as starting material through five steps of substitution, reduction, diazotization, esterification and alkaline hydrolysis-acidification. The obtained optimum conditions of reduction were n(4,4′-dinitrodiphenyl sulfide)∶n(hydrazine hydrate)=1∶3.03,amount of catalyst FeCl3 7% based on the weight of 4,4′-dinitrodiphenyl sulfide, reaction temperature 60～65 ℃ and reaction time 3 h. The final yield of 4, 4′-thiodibenzenethiol was about 50% with the purity of 99.5%.The structure of the product was confirmed by IR,GC-MS and 1H NMR.
Key words: 4,4′-thiodibenzenethiol; reduction; diazotization
收稿日期：2011-01-13
作者简介： 冯柏成（1965—），男，副教授.
