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有机化学
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有机化学 ›› 2003, Vol. 23 ›› Issue (3): 281-285. 上一篇    下一篇

研究论文

双缩二氨基硫脲类化合物的合成与结构

张安将;张力学;候云龙;熊轶;李贤均   

  1. 四川大学化学系;温州师范学院药物研究所
  • 发布日期:2003-03-25

Synthesis and Crystal Structure of Some Dithiocarbohydrazones

Zhang Anjiang;Zhang Lizue;Hou Yunlong;Xiong Yi   

  1. Department of Chemistry,Sichuan University;Institute of Pharmacy, Wenzhou Normal College
  • Published:2003-03-25

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694

被引次数

67 | 10

合成了1，5-二（4-甲氧基苯甲醛）双缩二氨基硫脲（1），1，5-二（对二甲 基氨基苯甲醛）双缩二氨基硫脲（2），1，5-二（2-呋喃甲醛）双缩二氨基硫脲（ 3）三个化合物，并通过元素分析、红外光谱、核磁共振、质谱进行了结构表征。 首次报道了双缩二氨基硫脲类化合物的^13C NMR数据，并发现在溶液中由于构象异 构体或二聚体的存在，该类化合物的部分^13C NMR谱峰出现矮而宽、不易检测的特 征。配体1形成的晶体为单斜晶系，具有P21/c空间群，a=1.4363(3)nm，b=1.2622 (2)nm，c=1.0970(2)nm，β=101.730（10）°，V=1.9472（6）nm^3，Z=4，Dc=1. 318g/cm^3，μ=0.193mm^-1，F(000)=816，R1=0.0560，ωR2=0.1496。由于分子间 弱氢键力的作用，在晶体中以二聚体的形式存在。

关键词: 缩氨基硫脲 P;晶体结构;二聚体;苯甲醛 P;甲氧基;元素分析;红外分光光度法, 核磁共振谱法;质谱法

Novel l,5-bis(4-methoxybenzaldehyde)-dithiocaibohydrazone (1), l,5- bis(p-dimethylaminobenzaldehyde)-dithiocarbohydrazone (2) and 1,5- bis ( 2-mraldehyde )-dithiocarbohydrazone (3) have been synthesized and characterized by elemental analysis, IR, NMR and MS spectra. The 13C NMR data of the dithiocarbohydrazones was initially reported. It was found that the partial~ 13C NMR signals of the title compounds presented small and broad, and were difficult to be detected as the result of different conformers or dimers formed in solution. The crystal structure of compound 1 was determined by X-ray single crystal diffraction analysis. Crystal structure of compound 1 belongs to monoclinic system with space P2-1/-c. The unit cell parameters are a = 1.4363(3) nm, b - 1.2622(2) nm, c = 1.0970(2) nm, β= 101.730 (10)°, K= 1.9472(6) nm~3, Z=4, D-c = 1.318 g/cm~3, // =0.193 mm~-1, F (OOO) = 816, R-1 =0.0560, W?2 = 0.1496.

Key words: THIOSEMICARBAZONE P;CRYSTAL STRUCTURE;DIMER;BENZALDEHYDE P, METHOXY GROUP;ELEMENTAL ANALYSIS;IR;1HNMR;MS

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