Synthesis and Crystal Structure of 5-Diazo-4-ethoxycarbonyl-3-methylthio Pyrazol |
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| Affiliation: | State Key Laboratory of Elemento-organic Chemistry, Institute of Elemento-organic Chemistry, Nankai University, Tianjin 300071, China;State Key Laboratory of Elemento-organic Chemistry, Institute of Elemento-organic Chemistry, Nankai University, Tianjin 300071, China;State Key Laboratory of Elemento-organic Chemistry, Institute of Elemento-organic Chemistry, Nankai University, Tianjin 300071, China |
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| Abstract: | The crystal of the title compound, 5-diazo-4-ethoxycarbonyl-3-methylthio pyrazole, has been prepared and determined by X-ray diffraction. The crystal belongs to the monoclinic system, space group C2/c with a = 29.174(8), b = 4.7592(12), c = 15.956(4) A, β =117.632(4)°, C7H8N4O2S, Mr = 212.23, V = 1962.7(9) A3, Z = 8, Dx = 1.436 g/cm3, S = 1.000,μ(MoKα) = 0.31 mm-1, T = 298(2) K, F(000) = 880, R = 0.0658 and wR = 0.1741 for 1091independent reflections with I ≥ 2σ(I). The crystal of the title compound is formed with π-πinteractions through electrostatic attractions. Moreover, no HSO4- exists in the crystal structure.Therefore, only diazo pyrazole was obtained rather than either diazonium salt of the corresponding pyrazole or diazoaminopyrazole when 5-amino-4-ethoxycarbonyl-3-methylthio pyrazole was diazotized with sodium nitrite, catalyzed by sulfuric acid at 0 ℃. |
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| Keywords: | 5-diazo-4-ethoxycarbonyl-3-methylthio pyrazole crystal structure diazotization |
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