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[1]刘安昌,李高峰,夏强,等.4，4’二巯基二苯硫醚的合成[J].武汉工程大学学报,2010,(03):25-27.
　LIU An chang,LI Gao fen,XIA Qiang,et al.Study on the synthesis of 4,4′ thiobis(Benzenethio1)[J].Journal of Wuhan Institute of Technology,2010,(03):25-27.
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4，4’二巯基二苯硫醚的合成(/HTML)
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《武汉工程大学学报》[ISSN:1674-2869/CN:42-1779/TQ]

卷:
期数:
2010年03期
页码:
25-27
栏目:
化学与化学工程
出版日期:
2010-03-31

文章信息/Info

Title:
Study on the synthesis of 4,4′ thiobis(Benzenethio1)
文章编号:
16742869(2010)03002503
作者:
刘安昌; 李高峰; 夏强; 张良
武汉工程大学湖北省新型反应器与绿色化学工艺重点实验室，湖北 武汉 430074
Author(s):
LIU Anchang;  LI Gaofen;  XIA Qiang;  ZHANG Liang
Hubei Key Lab of Novel Reactor and Green Chemical Technology,Wuhan Institute of Technology, Wuhan 430074, China
关键词:
4; 4’二巯基二苯硫醚;  磺化; 还原; 合成
Keywords:
4; 4′ Thiobis(benzenethio1);  sulfochlorination;  reduction
分类号:
O622
DOI:
-
文献标志码:
A
摘要:
以二苯硫醚为起始原料，经磺化、氯化和还原三步反应制得目的产物4，4’二巯基二苯硫醚.分别考察了各步反应的影响因素，确定反应的最佳工艺条件为n(二苯硫醚)：n(氯磺酸)：n(三氯氧磷)的摩尔配比为1∶2.3∶2.2，反应温度为100～110 ℃，反应时间为5 h.得产品4，4’一二氯磺酰二苯硫醚(2). n(锌粉):n(2)摩尔配比为9∶1，反应温度为70～80 ℃，反应时间为3 h，产物总收率60.1%.产物结构经IR与1H NMR证实.
Abstract:
4,4′ Thiobis(benzenethio1)(1)was synthesized by sulfochlorination and reduction with biphenyl sulfide as raw materials.and the reaction conditions were optimized．The optimum reaction conditions obtained were as follows：the molar ratio of n(HSO3Cl) ∶n(biphenyl sulfide)∶n(phosphorus oxychloride) is 1∶2.3∶2.2; reaction temperature was 100-110 ℃，reaction time was 5 h．The intermediate 4,4′ thiobis(benzenesulphonylchloride)(2)was abtained．Then the mixture of n(2)∶n(zinc dust)=1∶9 was reacted at 70-80 ℃ for 3 h to give (1) with a total yield of 60.1%. The structure of the product was confirmed by IR and 1H NMR

参考文献/References:

1］陆广，崔占臣，吕长利，等.新型含硫高折光指数光学树脂单体MPSDMA的合成及其共聚树脂的性能研究［J］. 高等学校化学学报,2001,22(6)：10361040.
［2］黎四芳，蔡兰珍.万能发泡剂OB SH的合成与应用［J］.化工时刊，2004，18（2）：910.
［3］Bert D B， Hong M， Dmitrii F. Synthesis and Characterization of Conjugated Mono andDithiol Oligomers and Characterization of TheirSelfAssembled Monolayers［J］. Langmuir, 2003,19：42724284.
［4］Katritzky A R, Rogers J W， Witek R M. Synthesis and Characterization of Blowing Agents and Hypergolics［J］. Journal of Energetic Materials, 2007,25：79109.
［5］Judek M. W, Spiewak B P. An efficient synthesis of thiobis(benzenethio1)［J］.Synthetic communications, 1998,28(2)：197199.

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备注/Memo

备注/Memo:
收稿日期：20091014作者简介：刘安昌(1964)，男，江西吉安人，教授,博士.研究方向：精细有机合成.
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