| 由季戊四醇合成季戊四硫醇的新方法 |
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| 引用本文： | 李长恭,祝勇,尚静艳,邓月娥,薛峰.由季戊四醇合成季戊四硫醇的新方法[J].光谱实验室,2013,30(5):2539-2542. |
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| 作者姓名： | 李长恭 祝勇 尚静艳 邓月娥 薛峰 |
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| 作者单位： | 河南科技学院化学化工学院 河南省新乡市华兰大道 453003 |
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| 基金项目： | 国家自然科学基金面上项目(21072046)资助;河南科技学院高学历人才资助项目 |
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| 摘 要： | 以季戊四醇为原料,先合成四对甲苯磺酸季戊四醇酯,然后四对甲苯磺酸季戊四醇酯与硫氰酸钾在N,N-二甲基甲酰胺中加热反应,生成了2,3,7,8-四硫螺4,4]壬烷,2,3,7,8-四硫螺4,4]壬烷经四氢化铝锂还原、酸化,得到季戊四硫醇.产物结构经熔点、红外光谱、质子核磁共振谱、拉曼光谱鉴定.
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| 关 键 词： | 季戊四硫醇 合成与表征 红外光谱 拉曼光谱 |
New Synthesis Method of 2,2-Bis (mercaptomethyl)-1,3-Propanedithiol From Pentaerythritol |
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| LI Chang-Gong
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ZHU Yong
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SHANG Jing-Yan
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DENG Yue-E
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XUE Feng.New Synthesis Method of 2,2-Bis (mercaptomethyl)-1,3-Propanedithiol From Pentaerythritol[J].Chinese Journal of Spectroscopy Laboratory,2013,30(5):2539-2542. |
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| Authors: | LI Chang-Gong ZHU Yong SHANG Jing-Yan DENG Yue-E XUE Feng |
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| Institution: | (College of Chemistry ＆. Chemical Engineering. Henan Institute of Science and Technology, Xinxiang 453003, P. R. China) |
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| Abstract: | 2,2-Bis （mercaptomethyl）- 1,3-propanedithiol was synthesized using pentaerythritol as raw materials. The synthetic route is mainly comprised of three steps. Pentaerythrityl benzenesulfonate was synthesized by pentaerythritol with 4-methylbenzenesulfonyl chloride in the presence of pyridine, and then it reacted with potassium thiocyanate in hot DMF to get 2,3,7,8-tetrasulfurwhorl4,4] nonane, which could be reduced by lithium aluminum hydride to pentaerythrithiol with a yield of 80% after acidification. The structure of synthesized compounds had been characterized by melting point,ill NMR,infrared spectroscopy and raman spectra. |
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| Keywords: | 2 2-Bis （mercaptomctryl）-l 3-Propanedithiol Synthesis and Characterization Infrared Spectroscopy Raman Spectra |
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