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新型硫代试剂((二甲基氨基-亚甲基)氨基)-3H-1,2,4-二噻唑-3-硫酮的合成工艺研究

Study on Synthesis of New-sulfurizing Reagent DDTT
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摘要 以四氢呋喃(THF)为溶剂,采用易得的5-氨基-1,2,4-二噻唑-3-硫酮(氢化黄原素)和N,N-二甲基甲酰胺二甲基缩醛为原料合成((二甲基氨基-亚甲基)氨基)-3 H-1,2,4-二噻唑-3-硫酮(DDTT)。通过对影响收率的关键因素进行研究,找到了最佳反应条件:n(氢化黄元素)∶n(N,N-二甲基甲酰胺二甲基缩醛)为1∶1.1,25℃下反应6h,收率达90%。合成工艺操作方便,纯化简单,收率高。 ((Dimethylamino-methylidene)amino)-3H-1,2,4-dithiazoline-3-thione was synthesized from 5-a- mino-3H-1,2,4-dithiazole-3-thione (xanthane hydride) using THF as solvent. The experimental results showed that the optimum conditions were as follows, the molar ratio was 1 ~ 1.1, the reaction temparature was 25℃and the reaction time was 6 h. The yield was 90%. Convenient operation of the process, easy of the product purification up, high yield and low pollution show that the process is suitable for industrial production, and it opens wide prospects for market application.
出处 《化学世界》 CAS CSCD 北大核心 2013年第12期734-736,739,共4页 Chemical World
基金 2011年盐城市科技计划项目(YK2011124)
关键词 ((二甲基氨基一亚甲基)氨基)-3H-1 2 4-二噻唑-3-硫酮 硫代试剂 氢化黄原素 N N-二甲基甲酰胺二甲基缩醛 ((dimethylamino-methylidene) amino) 3 H-1, 2, 4-dithiazoline-3-thione sulfurizing reagent xanthane hydride~ N, N- dimethylformamide dimethyl acetal
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