Redetermination of the structure of 2-amino-8-thia-1,5-di-aza-spiro-[4.5]dec-1-en-5-ium chloride monohydrate

2-氨基-8-硫杂-1,5-二氮杂螺-[4.5]癸-1-烯-5-氯化物一水合物结构的重新测定

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作者:Lyudmila A Kayukova, Elmira M Yergaliyeva, Anna V Vologzhanina

Abstract

The reaction of β-(thio-morpholin-1-yl)propio-amidoxime with tosyl chloride in CHCl3 in the presence of DIPEA when heated at 343 K for 8 h afforded the title hydrated salt, C7H14N3S+·Cl-·H2O, in 84% yield. This course of the tosyl-ation reaction differs from the result of tosyl-ation obtained for this substrate at room temperature, when only 2-amino-8-thia-1,5-di-aza-spiro-[4.5]dec-1-ene-5-ammonium tosyl-ate was isolated in 56% yield. The structure of the reaction product was established by physicochemical methods, spectroscopy, and X-ray diffraction. The single-crystal data demonstrated that the previously reported crystal structure of this compound [Kayukova et al. (2021). Chem. J. Kaz, 74, 21-31] had been refined in a wrong space group. In the extended structure, the chloride anions, water mol-ecules and amine groups of the cations form two-periodic hydrogen-bonded networks with the fes topology.

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