全文下载:2012060560
冯柏成, 李同全, 张庆云
(青岛科技大学 化工学院, 山东 青岛 266042)
摘要: 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4.5 h。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1H NMR进行了确证。
关键词: 4-苯硫基苯酚; 对硝基氯苯; 重氮化
中图分类号: TQ 247.2文献标志码: A
Preparation and Characterization of 4-Thiophenylphenol
FENG Bai-cheng, LI Tong-quan, ZHANG Qing-yun
(College of Chemical Engineering, Qingdao University of Science and Technology, Qingdao 266042,China)
Abstract: 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.
Key words: 4-thiophenylphenol; 4-nitrochlorobenzene; diazotization
收稿日期:2012-01-05
作者简介:冯柏成(1965—),男,副教授.