高等学校化学学报 ›› 2004, Vol. 25 ›› Issue (12): 2278.

• 研究论文 • 上一篇    下一篇

2-乙氨基-6H-5-(1-苯基-3-甲基/苯基-5-吡唑啉酮-4-基)-1,3,4-噻二嗪的合成和晶体结构

彭邦华1, 刘广飞1, 刘浪1, 贾殿赠1, 郁开北2   

  1. 1. 新疆大学应用化学研究所, 乌鲁木齐830046;
    2. 中国科学院成都分院分析测试中心, 成都610041
  • 收稿日期:2003-10-29 出版日期:2004-12-24 发布日期:2004-12-24
  • 基金资助:

    国家自然科学基金(批准号:20161003)资助

Synthesis and Crystal Structure of 2-Ethylamino-6H-5-(1-phenyl-3- methyl/phenyl-5-pyrazolone-4-ylene)-1,3,4-Thiadiazine

PENG Bang-Hua1, LIU Guang-Fei1, LIU Lang1, JIA Dian-Zeng1, YU Kai-Bei2   

  1. 1. Institute of Applied Chemistry, Xinjiang University, Urumqi 830046, China;
    2. Analytical Center, Chengdu Branch of Chinese Academy of Sciences, Chengdu 610041, China
  • Received:2003-10-29 Online:2004-12-24 Published:2004-12-24

摘要: 利用1-苯基-3-甲基/苯基-4-氯乙酰基-吡唑啉酮-5(PMCP/DPCP)与4-乙基氨基硫脲(ETSC)发生缩合反应,生成了2个新的双杂环化合物2-乙氨基-6H-5-(1-苯基-3-甲基/苯基-5-吡唑啉酮-4-基)-1,3,4-噻二嗪(PMCP-ETSC/DPCP-ETSC),并对其进行元素分析、红外光谱、核磁共振表征和晶体结构分析.PMCP-ETSC晶体属于单斜晶系,Pm空间群,晶胞参数:a=0.7947(1)nm,b=0.8348(1)nm,c=1.1990(2)nm,β=106.07(1)°,V=0.77269(2)nm3,Z=2,Dc=1.356g/cm3,μ=0.219mm-1,F(000)=332,R=0.0298,wR=0.0704.该化合物通过分子间氢键形成沿c轴无限延伸的一维链状结构.DPCP-ETSC晶体属于正交晶系,Pna21空间群,晶胞参数:a=1.1478(2)nm,b=1.3545(2)nm,c=1.1994(2)nm,V=1.8646(4)nm3,Z=4,Dc=1.345g/cm3,μ=0.194mm-1,F(000)=792,R=0.0345,wR=0.0694,此化合物通过分子间氢键形成沿c轴成链状,沿ab平面成波浪状的超分子结构.

关键词: 缩合反应, 杂环, 晶体结构, 超分子结构

Abstract: Two novel pyrazolone derivatives 2-ethylamino-6H-5-(1-phenyl-3-methyl/phenyl-5-pyrazolone-4-ylene)-1,3,4-thiadiazine(PMCP-ETSC/DPCP-ETSC)containing NNS six-membered heterocycles were synthesized by the condensation reaction of 1-phenyl-3-methyl/phenyl-4-chloroacetyl-pyrazolone-5 with 4-ethylthiosemicarbazide. The title compounds were characterized by elemental analysis, IR, 1H NMR, 13C NMR and single-crystal X-ray diffraction. The crystal structure of PMCP-ETSC belongs to the monoclinic system, space group Pm with the lattice parameters a= 0.794 7(1) nm, b= 0.834 8(1) nm, c=1.199 0(2) nm, β=106.07(1)°, V=0.772 69(2) nm3, Z=2, Dc=1.356 g/cm3, μ=0.219 mm-1, F(000)=332, R=0.029 8, wR=0.070 4. The X-ray analysis showed that one-dimentional concatenate structure was formed along the c axis by the intermolecular hydrogen bonds. The crystal of DPCP-ETSC belongs to the orthorhombic system, space group Pna2 1, and its lattice parameters are as follows: a=1.147 8(2) nm, b=1.354 5(2) nm, c= 1.199 4(2) nm, V=1.864 6(4) nm3, Z=4, Dc=1.345 g/cm3, μ=0.194 mm-1, F(000)=792, R=0.034 5, wR= 0.069 4. The intermolecular hydrogen bonds led to the formation of chain-like one-dimensional compound along c axis and extended along ab plane to form the wave-like supramolecular structure.

Key words: Condensation reaction, Heterocycles, Crystal structure, Supramolecular structure

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