| Synthesis and Crystal Structure of o-Methylisourea Hydrosulfate |
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| 作者姓名： | 杨晓兰 罗宗伟 成禹杉 林琳 余瑜 |
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| 作者单位： | Key Laboratory of Biochemistry and Molecular Pharmacology of Chongqing Laboratory of Pharmaceutical Chemistry and Biomaterials，Chongqing School of Pharmaceutical Sciences，Chongqing University of Medical Sciences，Key Laboratory of Biochemistry and Molecular Pharmacology of Chongqing Laboratory of Pharmaceutical Chemistry and Biomaterials，Chongqing School of Pharmaceutical Sciences，Chongqing University of Medical Sciences，Key Laboratory of Biochemistry and Molecular Pharmacology of Chongqing Laboratory of Pharmaceutical Chemistry and Biomaterials，Chongqing School of Pharmaceutical Sciences，Chongqing University of Medical Sciences，Key Laboratory of Biochemistry and Molecular Pharmacology of Chongqing Laboratory of Pharmaceutical Chemistry and Biomaterials，Chongqing School of Pharmaceutical Sciences，Chongqing University of Medical Sciences，Key Laboratory of Biochemistry and Molecular Pharmacology of Chongqing Laboratory of Pharmaceutical Chemistry and Biomaterials，Chongqing School of Pharmaceutical Sciences，Chongqing University of Medical Sciences，Chongqing 400016 China，Chongqing 400016 China，Chongqing 400016 China，Chongqing 400016 China，Chongqing 400016 China |
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| 基金项目： | This work was supported by the National Natural Science Foundation of China (Nos. 30171070 and 30371632) |
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| 摘 要： | l INTRODUCTION As an important and capital intermediate of chemi- cal engineering, medicine and pesticide, o-methyli- sourea today is mainly used to synthesize fluoracil antitumor drugs, pesticides and polyantibacterials. According to the applications and syntheses, o- methylisourea is usually prepared as its salts and es- ters, such as o-methylisourea hydrosulfate, o-me- thylisourea sulfate, o-methylisourea acetate, o-methy- lisourea formate, and so on, since o-methylisourea is unstable.…
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| 关 键 词： | O-甲基异脲硫酸化物 合成路线 晶体结构 X-射线衍射 化学分析 |
Synthesis and Crystal Structure of o-Methylisourea Hydrosulfate |
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| YANG Xiao-Lan,LUO Zong-Wei,CHENG Yu-Shan,LIN Lin,YU Yu.Synthesis and Crystal Structure of o-Methylisourea Hydrosulfate[J].Chinese Journal of Structural Chemistry,2006,25(3):290-294. |
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| Authors: | YANG Xiao-Lan LUO Zong-Wei CHENG Yu-Shan LIN Lin YU Yu |
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| Institution: | Key Laboratory of Biochemistry and Molecular Pharmacology of Chongqing, Laboratory of Pharmaceutical Chemistry and Biomaterials,Chongqing School of Pharmaceutical Sciences,Chongqing University of Medical Sciences, Chongqing 400016, China |
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| Abstract: | To determine the structure of o-methylisourea for instructing its application and factory production, crystalline o-methylisourea hydrosulfate was synthesized in this paper by methylation of urea with dimethylsulfate, followed by acidification in 53% yield. Its single crystal prepared from 95% ethanol is determined by X-ray diffraction analysis. The crystal is of monoclinic, space group P21/c with a = 8.5330(10), b = 7.0548(9), c = 11.6764(14)(A), β = 95.429(2)°, Mr = 172.16, V = 699.75(15)(A)3, Dc = 1.634 g/cm3, Z = 4, F(000) = 360 and μ(MoKα) = 0.435 mm-1. Of 1511 unique reflections, 1294 is gotten (I > 2σ(I)). The structure was solved by Fourier method and refined to R = 0.0438 and wR = 0.1209. The crystal structure shows that o-methylisourea combines with bisulfate via the intramolecular hydrogen bond between N(2)-H(4) of o-methylisourea and O(2) of bisulfate. As a result, the molecular structure is H2NC(OCH3)NH2]HSO4 and the formula is C2H8N2O5S or C2H7N2O·HSO4 but not H2NC(OCH3)NH·HSO4 or H2NC(OCH3)NH·0.5H2SO4. |
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| Keywords: | O-methylisourea hydrosulfate synthesis crystal structure X-ray diffraction |
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