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

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.