由季戊四醇合成季戊四硫醇的新方法  

New Synthesis Method of 2,2-Bis(mercaptomethyl)-1,3-Propanedithiol From Pentaerythritol

作　　者：李长恭[1] 祝勇[1] 尚静艳[1] 邓月娥[1] 薛峰[1] 

机构地区：[1]河南科技学院化学化工学院,河南省新乡市华兰大道453003

出　　处：《光谱实验室》2013年第5期2539-2542,共4页Chinese Journal of Spectroscopy Laboratory

基　　金：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(08009)资助

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。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-tetrasulfurwhorl[4,4] 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.

关 键 词：季戊四硫醇 合成与表征 红外光谱 拉曼光谱 

分 类 号：O657.61[理学—分析化学]