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Abstract <p>In this study, a two-step synthetic procedure was developed for preparing the target perhalogenated dihydroxy derivatives of an apically substituted <i>closo</i>-decaborate anion. In the first step, complete halogenation of the starting bis-DMF derivative 1,10-B<sub>10</sub>H<sub>8</sub>(OCHNMe<sub>2</sub>)<sub>2</sub> was achieved using sulfuryl chloride or elemental bromine in dichloromethane under an inert atmosphere. This allowed for the replacement of all residual hydrogen atoms in the boron framework with halogens without affecting the DMF substituents. In the second step, hydrolytic cleavage of the O–C bond in the perhalogenated <i>closo</i>-decaborane derivatives was performed to form dihydroxy derivatives of the <i>closo</i>-decaborate anion. The process was carried out in a water-ethyl alcohol mixture at 80°C for 4 h using hydrazine hydrate and tetrabutylammonium hydroxide to complete the conversion. The obtained compounds were characterized by physicochemical analytical methods. Compounds 1,10-B<sub>10</sub>Br<sub>8</sub>(OCHNMe<sub>2</sub>)<sub>2</sub> and (Bu<sub>4</sub>N)<sub>2</sub>[1,10-B<sub>10</sub>Br<sub>8</sub>(OH)<sub>2</sub>] were studied by X-ray diffraction methods.</p>

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Two-Step Synthesis of Perhalogenated Dihydroxy Derivatives of Apically Substituted closo-Decaborate Anions

  • 期刊论文

  • 发表日期：

    2025年12月1日

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  • E. S. Turyshev,
  • A. V. Golubev,
  • A. S. Kubasov,
  • P. A. Starodubets,
  • V. A. Mantsireva,
  • S. Z. Popovich,
  • A. S. Gracheva,
  • A. Yu. Bykov,
  • K. Yu. Zhizhin,
  • N. T. Kuznetsov

摘要

Abstract

In this study, a two-step synthetic procedure was developed for preparing the target perhalogenated dihydroxy derivatives of an apically substituted closo-decaborate anion. In the first step, complete halogenation of the starting bis-DMF derivative 1,10-B10H8(OCHNMe2)2 was achieved using sulfuryl chloride or elemental bromine in dichloromethane under an inert atmosphere. This allowed for the replacement of all residual hydrogen atoms in the boron framework with halogens without affecting the DMF substituents. In the second step, hydrolytic cleavage of the O–C bond in the perhalogenated closo-decaborane derivatives was performed to form dihydroxy derivatives of the closo-decaborate anion. The process was carried out in a water-ethyl alcohol mixture at 80°C for 4 h using hydrazine hydrate and tetrabutylammonium hydroxide to complete the conversion. The obtained compounds were characterized by physicochemical analytical methods. Compounds 1,10-B10Br8(OCHNMe2)2 and (Bu4N)2[1,10-B10Br8(OH)2] were studied by X-ray diffraction methods.