Synthesis and Crystal Structural Characterization of a Thiosemicarbazone Derived from 4-Acylpyrazolone  

作　　者：LIU Guang-Fei LIU Lang HU Xin JIA Dian-Zeng YU Kai-Bei 

机构地区：[1]Institute of Applied Chemistry, Xinjiang University, Urumqi 830046, China [2]Chengdu Institute of Organic Chemistry, The Chinese Academy of Sciences, Chengdu, Sichuan 610041, China

出　　处：《Chinese Journal of Structural Chemistry》2006年第10期1233-1237,共5页结构化学（英文）

基　　金：This project was supported by the National Natural Science Foundation of China (No. 20462007) and Xinjiang Bureau of Education (No. XJEDU2004S06)

摘　　要：The reaction of 4-（p-fluobenzoyl）-2,5-dihydro-3-methyl-1-phenyl pyrazol-5-one with thiosemicarbazide in MeOH followed by recrystallization in EtOH gave rise to yellowish lamellar crystals of 4（p-fluo-a-aminothiocarbonyl hydrazonobenzal）-2,5-dihydro-3-methyl- 1-phenyl pyrazol-5-one 1. It crystallizes in orthorhombic, space group Pbca with a = 18.445（4）, b = 11.987（2）, c = 19.249（4） °A,, V= 4256.1（18）°A^3, Z = 8, Mr = 415.49, Dc= 1.297 g/cm^3, T = 296（2） K, F（000） = 1744,μ（MoKα） = 0.186 cm^-1, R = 0.0521 and wR = 0.1211 for 1661 observed reflections with I 〉 2σ（I）. The compound was structurally characterized by elemental analyses, IR and ^1H NMR. The intermolecular hydrogen bonds are present and a two-dimensional framework is formed by two intermolecular hydrogen bonds in the （001） plane.The reaction of 4-（p-fluobenzoyl）-2,5-dihydro-3-methyl-1-phenyl pyrazol-5-one with thiosemicarbazide in MeOH followed by recrystallization in EtOH gave rise to yellowish lamellar crystals of 4（p-fluo-a-aminothiocarbonyl hydrazonobenzal）-2,5-dihydro-3-methyl- 1-phenyl pyrazol-5-one 1. It crystallizes in orthorhombic, space group Pbca with a = 18.445（4）, b = 11.987（2）, c = 19.249（4） °A,, V= 4256.1（18）°A^3, Z = 8, Mr = 415.49, Dc= 1.297 g/cm^3, T = 296（2） K, F（000） = 1744,μ（MoKα） = 0.186 cm^-1, R = 0.0521 and wR = 0.1211 for 1661 observed reflections with I 〉 2σ（I）. The compound was structurally characterized by elemental analyses, IR and ^1H NMR. The intermolecular hydrogen bonds are present and a two-dimensional framework is formed by two intermolecular hydrogen bonds in the （001） plane.

关 键 词：pyrazol-5-one thiosemicarhazide crystal structure SYNTHESIS 

分 类 号：O623.8[理学—有机化学] O623.7[理学—化学]