N-甲基-N-哌嗪基二硫代氨基甲酸锑的合成与表征  

Synthesis and Characterization of N′-Methyl-N-piperazinyl-carbodithioato-S,S′-antimony

作　　者：杨小兰[1] 钟国清[1] 张志朋[1] 张艳[1] 

机构地区：[1]西南科技大学四川省非金属复合与功能材料重点实验室-省部共建国家重点实验室培育基地,四川绵阳621010

出　　处：《精细化工》2012年第4期357-360,共4页Fine Chemicals

基　　金：四川省教育厅重点科研项目(10ZA016)~~

摘　　要：用CS2、N-甲基哌嗪和Sb2O3为原料,在三氯甲烷中合成了N-甲基-N-哌嗪基二硫代氨基甲酸锑(Ⅲ)配合物[Sb(S2CNC4H8NCH3)3]H2O,用化学分析、元素分析、红外光谱、X射线粉末衍射、热分析等手段对配合物的组成和结构进行了表征,探索了反应时间、反应温度、不同溶剂对产率的影响。结果表明,以三氯甲烷为溶剂,25℃反应1 h,用CHCl3-CH3OH混合溶剂重结晶后产率最高,可达74%。The complex of N′-methyl-N-piperazinyl-carbodithioato-S,S′-antimony（Ⅲ） was synthesized with the raw materials of carbon bisulfide,N-methyl-piperazinyl and antimonous oxide in chloroform.The composition and structure of the complex was characterized by means of chemical and elemental analysis,fourier transformed infrared spectra（FTIR）,X-ray powder diffraction（XRD） and thermal analysis.The results show that the composition of the complex is [Sb（S2CNC4H8NCH3）3]H2O,and the ligand is coordinated simultaneously with Sb（Ⅲ） via the sulphur atoms of dithiocarbamate to form bidentate chelates.The effects of reaction temperature,reaction time and different solvent on the yield were discussed respectively.The results showed that the yield of the complex reached a maximum of 74% when chloroform was used as the solvent at 25 ℃ for 1 h,and the mixed solvent of chloroform-methanol was used in recrystallization.

关 键 词：锑(Ⅲ)配合物 N-甲基哌嗪 氨荒酸盐 医药与日化原料 

分 类 号：TQ265.2[化学工程—有机化工] O627.52[理学—有机化学]