【摘 要】
：
To determine the structure of o-methylisourea for instructing its application and factory production, crystalline o-methylisourea hydrosulfate was synthesized i
【机 构】
：
Key Laboratory of Biochemistry and Molecular Pharmacology of Chongqing
【基金项目】
：
the National Natural Science Foundation of China
论文部分内容阅读
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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