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=y=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.
参考文献
| [1] | HUANG Zhishu,WU Xiaolin,LIU Yu,et al.The Synthesis and Biological Activity of Alkyl 4-Aryl-3-Thio-Allophanate[J].ChineseJ Org Chem,1998,18(5):481-485(in Chinese).黄志纾,吴晓琳,刘煜,等.硫脲类衍生物及其生物活性研究[J].有机化学,1998,18(5):481-485. |
| [2] | HUANG Jie,SONG Jirong,REN Yinghui,et al.Preparation,Crystal Structure and Theoretical Calculation of 4,6-Dimethoxy-2-(methoxycarbamidothiocarbamido) pyrimidine[J].Acta Chim Sin,2006,64(1):9-16(in Chinese).黄洁,宋纪蓉,任莹辉,等.4,6-二甲氧基-2-[甲氧脲基硫代脲基]嘧啶的合成、晶体结构和理论计算[J].化学学报,2006,64(1):9-16. |
| [3] | SUN Xiaohong,GAO Runli,LIU Yuanfa,et al.Synthesis of Alkyl-4-Aryl-3-Thio-Allophanate[J].Chem Eng,2003,31(2):75-77(in Chinese).孙晓红,高润利,刘源发,等.硫脲类化合物杀菌剂的合成[J].化学工程,2003,31 (2):75-77. |
| [4] | SHI Qing,LI Liang.Recent Advances in Biological Activity of Acylthiourea Compounds[J].Guangzhou Chem Ind,2010,38(8):55-58(in Chinese).石青,李良.酰脲类化合物的生物活性研究进展[J].广州化工,2010,38(8):55-58. |
| [5] | LI Yingjun,ZHANG Zhiguang,JIN Kun,etal.Synthesis,Characterization and Biological Activity of Acylthiourea Derivatives[J].Acta Chim Sin,2007,65(9):834-840(in Chinese).李英俊,张治广,靳焜,等.酰基硫脲衍生物的合成、结构表征及生物活性研究[J].化学学报,2007,65(9):834-840. |
| [6] | LIN Qi,WEI Taibao,YAO Hong,et al.Studies on the Weak Interaction and Supramolecular Structure in the Crystal of N-Ethoxycarbonyl-N′-Arylthiourea[J].Acta Chim Sin,2007,65(2):159-164(in Chinese).林奇,魏太保,姚虹,等.N-乙氧羰基-N′-取代芳基硫脲晶体中的弱相互作用及超分子结构研究[J].化学学报,2007,65(2):159-164. |
| [7] | PENG Hao,HE Hongwu.Synthesis,Crystal Structure and Biological Activity of N-Substituted Benzoyl-N′-Substituted Arylthiourea[J].Chinese J Org Chem,2007,27(4):502-506(in Chinese).彭浩,贺红武.N-取代苯甲酰基-N′-取代芳基硫脲的合成、晶体结构及生物活性[J].有机化学,2007,27(4):502-506. |
| [8] | WANG Daxiang,BO Zaisu.New Pesticide Series[M].Wuhan:Central China Normal University Press,1998:31 (in Chinese).王大翔,柏再苏.新农药论丛[M].武汉:华中师范大学出版社,1998:31. |
| [9] | XIAN Liang,ZHANG Fengzhen,LIN Xin.Research of Bioactivities of Thiourea Derivatives and Their Complexes[J].JNorthwest Univ Nat(Nat Sci),2010,31(2):7-11 (in Chinese).鲜亮,张峰振,林欣.硫脲衍生物及其配合物的生物活性研究进展[J].西北民族大学学报(自然科学版),2010,31(2):7-11. |
| [10] | XUE Sijia,SHEN Jiefeng,CAI Zhijuan,et al.N-(1-Ethoxycarbonylalkyl)-N′-β-pyridylcarbonylthiourea[J].Chinese J Org Chem,2007,27(9):1137-1141(in Chinese).薛思佳,申杰峰,蔡志娟,等.N-乙氧羰基取代甲基-N′-β-吡啶甲酰硫脲的合成及晶体结构[J].有机化学,2007,27(9):1137-1141. |
| [11] | LIU Wukun,ZHOU Jinpei,ZHANG Tong,et al.Design and Synthesis of Thiourea Derivatives Containing a Benzo[5,6]cyclohepta[1,2-b]pyridine Moiety as Potential Antitumor and Anti-inflammatory Agents[J].Bioorg Med Chem Lett,2012,22:2701-2704. |
| [12] | HU Jinghan,XU Weixia,WEI Taibao.Studies on the Anion Recognition of N-Aryl-N′-(4-Ethyloxybenzoyl) Thioureas Derivatives by Spectroscopy[J].Spectrosc Spear Anal,2007,27(6):1172-1175(in Chinese).胡京汉,徐维霞,魏太保.N-芳基-N′-(4-乙氧基苯甲酰基)硫脲衍生物阴离子识别性能的光谱研究[J].光谱学与光谱分析,2007,27(6):1172-1175. |
| [13] | SHI Daqing,WANG Haiying,YANG Fang,et al.Synthesis of Anion Receptors Basedon Aroyithiourea and Their Anion Recognition[J].Acta Chim Sin,2007,65(16):1713-1717(in Chinese).史达清,王海营,杨芳,等.芳酰基硫脲受体的合成及对阴离子识别研究[J].化学学报,2007,65(16):1713-1717. |
| [14] | QIN Gaofei,ZHOU Ying,LUO Qin,et al.Process and Application of Recovering Platinum from Used Liquid-phase Catalysts by Solvent Extraction with Thiourea[J].Chinese J Appl Chem,2011,28(11):1337-1339 (in Chinese).秦高飞,周莹,罗芩,等.液相废催化剂中铂的硫脲萃取回收工艺及应用[J].应用化学,2011,28(11):1337-1339. |
| [15] | LIN Qi,WANG Yalin,WEI Taibao,et al.Studies on Synthesis of N-Ethoxylcarbonyl-N′-nitrophenylamide-thioureas and Their Anion Recognition Abilities[C]//The National Symposium on the Fourteenth Macrocyclic Chemistry and the Sixth Supramolecular Chemistry.Lanzhou:Northwest Normal University,2008:651-652(in Chinese).林奇,王雅琳,魏太保,等.N-乙氧羰基-N′-硝基苯基胺基硫脲的合成及其阴离子识别性能[C]//全国第十四届大环化学暨第六届超分子化学学术讨论会论文集.兰州:西北师范大学,2008:651-652. |
| [16] | Sheldrick G M.SHELXS-97:Program for Crystal Structure Re-finement,Gottingen University,Gottingen,1997. |
| [17] | SONG Jirong,REN Yinghui,HUANG Jie,et al.Synthesis,Crystal Structure and Theoretical Calculation of 4-(1,2,4-Triazole-5-one-4-yl)-3-thiourea Carboxylic Acid Ethyl Ester[J].Acta Chim Sin,2006,64(13):1334-1340(in Chinese).宋纪蓉,任莹辉,黄洁,等.4-(1,2,4-三唑-5-酮-4-基)-3-硫代脲酸乙酯的合成、晶体结构及理论计算[J].化学学报,2006,64(13):1334-1340. |
| [18] | Zhao D,Huang J,Song J R,etal.Synthesis,Crystal Structure and Thermal Analysis of N-(2,3-Dimethyl-phenyl)-N′-(methoxyl formyl) thiourea[J].Chem Res Chinese Univ,2012,28(2):230-233. |
| [19] | ZHANG Xinyu,ZHANG Pengjuan,SONG Jirong,et al.Synthesis,Crystal Structure,Theoretical Calculation,Specific Heat Capacity and Thermodynamic Properties of 4-[(3-Ethoxyacyl-2-thio) thiourea]-4′-[(3-etoxyacyl-2-thio)thiourea]diphenyloxide[J].Acta Chim Sin,2010,68(17):1692-1698(in Chinese).张新瑜,张鹏娟,宋纪蓉,等.4-[(3-乙氧酰基-2-硫代)硫脲]4′-[(3-乙氧酰基-2-硫代)硫脲]二苯醚配体的制备、晶体结构、量化计算、比热容、热力学性质研究[J].化学学报,2010,68(17):1692-1698. |
| [20] | Zhang X Y,Huang J,Song J R,et al.Synthesis,Crystal Structure,Theoretical Calculation,Specific Heat Capacity,and Thermodynamic 4,4′-Bis(3-N-methoxyformyl thioureido)-diphenyloxide[J].Chinese J Chem,2010,28:1897-1901. |
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