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N-(乙氧酰基)-N’-(2,4-二硝基苯胺基)硫脲的合成、晶体结构、比热容及热力学性质

何建云1,黄洁1*,宋纪蓉1,2,赵毅莎1,马聪1,徐抗震1   

  1. (1.西北大学化工学院，陕西省物理无机化学重点实验室 西安 710069；2.故宫博物院文保科技部 北京 100009)
  • 收稿日期:2012-09-12 修回日期:2012-11-20 出版日期:2013-07-10 发布日期:2013-07-10
  • 通讯作者: 黄洁，副教授; Tel:029-88307755; Fax:029-88302633; E-mail:huangjie@nwu.edu.cn; 研究方向：新型硫脲类杀菌剂的合成
  • 基金资助:
    国家自然科学基金（20571060）陕西省自然科学基金（2007B08）陕西省农业科技攻关计划项目(S2013NY2884)资助项目

Synthesis, Crystal Structure, Specific Heat Capacity and Thermodynamic Properties of N-(Ethoxycarbonyl acyl)-N'-(2,4-dinitrophenyl amino) Thiourea

HE Jianyun1, HUANG Jie1*, SONG Jirong1,2, ZHAO Yisha1, MA Cong1, XU Kangzhen1   

  1. (1.Department of Chemical Engineering/Shaanxi Key Laboratory of Physico-Inorganic Chemistry,Northwest University,Xi′an 710069,China;
    2.Conservation Technology Department,the Palace Museum,Beijing 100009,China)
  • Received:2012-09-12 Revised:2012-11-20 Published:2013-07-10 Online:2013-07-10

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摘要： 以PEG-400为催化剂，利用氯甲酸乙酯和硫氰酸钾反应生成的乙氧酰基异硫氰酸酯为中间体与2,4-二-硝基苯肼反应，得到N-(乙氧酰基)-N′-(2,4-二硝基苯胺基)硫脲，通过IR、元素分析等方法对其结构进行了表征。 在室温条件下，采用缓慢挥发法培养出适合用于X射线衍射测试的单晶。 晶体结构数据表明，晶体属单斜系，P2(1)/c空间群，晶胞参数:a=4.1919(2) nm,b=12.295(6) nm,c=23.828(11) nm,α=γ=90.00°,β=92.467(10)°,V=14397(12),Dc=1.519 g/cm3,μ=0.263 cm-1,F(000)=680,Z=4,R1=0.1121,wR2=0.2540。 并对标题化合物进行了热重分析和比热容测定，计算了热力学函数；证明该化合物有良好的热稳定性。

关键词: 合成, X单晶衍射, 晶体结构, 比热容, 热力学性质

Abstract: N-(Ethoxycarbonyl acyl)-N′-(2,4-dinitrophenyl amino) thiourea was synthesized using 2,4-dinitrophenylhydrazine, potassium thiocyanate and ethyl chloroformate as precursors in ethyl acetate in the presence of Macrogol-400 catalyst. The structure was characterized by elemental analysis and FI-IR. Single crystal of the title compound was obtained by slowly evaporating solvents at the room temperature. The crystal structure was determined with single crystal X-ray diffractometer. Crystal data are: monoclinic, P2(1)/c space group, a=4.1919(2) nm, b=12.295(6) nm, c=23.828(11) nm, α=γ=90.00°, β=92.467(10)°, V=1439.7(12), Dc=1.519 g/cm3, μ=0.263 cm-1, F(000)=680, Z=4, R1=0.1121, wR2=0.2540. The thermal behavior of the title compound was studied under a non-isothermal condition by DSC method. The specific heat capacity of the title compound was determined with continuous Cp mode of mircocalorimeter. The structure analysis and thermodynamic properties proved that the title compound has good stability, which is good for transportation and storage.

Key words: synthesis, X-ray diffraction, crystal structure, Specific Heat Capacity, thermodynamic properties

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