1-苯基-3-甲基-4-(6-氢-4-甲基氨基-5-硫杂-2,3-吡嗪)-吡唑啉酮的合成与晶体结构

通过1-苯基-3-甲基-4-氯乙酰基-吡唑啉酮-5 (PMCP) 和4-甲基氨基硫脲 (MTSC) 缩合, 形成了一种新的双杂环化合物 (PMCP-MTSC)。利用元素分析与单晶X-射线衍射进行了表征。 该化合物(C14H15N5OS)属单斜晶系, P21 空间群, 晶体学参数为 a = 7.634(1), b = 11.639(2), c = 8.150(2) ? ?= 98.13(1), V = 716.9(2) ?, Z = 2, Dc = 1.396 g/cm3, (MoKa) = 0.232 mm-1, F(000) = 316, Mr = 301.37。结构由直接法解出,共收集3114个衍射点,其中I > 2(I)的独立衍射点有2453个,用全矩阵最小二乘法修正,最终偏离因子:R = 0.0294, wR = 0.0738。结构分析表明: 该化合物以酮式存在,分子间通过氢键作用(N(5)H…O)连接起来并形成一维链状结构。

Synthesis and Crystal Structure of 1-Phenyl-3-methyl-4-(6-hydro-4-methylamino-5-sulfo-2,3-pyrazine)-pyrazole-5-one

A novel pyrazolone derivate (PMCP-MTSC) containing NNS hexa-atomic heterocycle was obtained by the reaction of 1-phenyl-3-methyl-4-chloroacetyl-pyrazolone-5 with 4-methyl thiosemicarbazine. The title compound has been characterized by elemental analysis and single-crystal X-ray diffraction. The crystal belongs to monoclinic system, space group P21 with the following unit cell parameters: a = 7.634(1), b = 11.639(2), c = 8.150(2) ? ?= 98.13(1), V = 716.9(2) ?, Z = 2, Dc = 1.396 g/cm3, (MoK) = 0.232 mm-1, F(000) = 316, Mr = 301.37, R = 0.0294 and wR = 0.0738. The crystal structure was determined by direct methods and refined by full-matrix least-squares techniques. The structure analyses show the title compound is the keto form. One dimensional chain structure was formed by the intermolecular hydrogen bonds (N(5)H…O).