N-tert-butoxycarbonyl (BOC) protected [V₆O₁₃{(OCH₂)₃CNH₂}₂]²⁻: synthesis, structural characterization, and solution behavior

Abstract

Herein, we report the synthesis of N-tert-butoxycarbonyl (BOC) protected [V₆O₁₃{(OCH₂)₃C–NH₂}₂]²⁻ built from the Lindqvist-type hexavanadate. The reaction of di-tert-butyl dicarbonate (BOC₂O) with tris(hydroxymethyl)aminomethane (Tris) led to the organic derivative [(OCH₂)₃C–NH(BOC)] that reacts with the decavanadate in dimethylacetamide (DMA) to form the [V₆O₁₃{(OCH₂)₃ C–NH(BOC)}₂]²⁻ anion. The tetrabutylammonium (TBA⁺) salt of this hybrid polyoxovanadate, TBA₂[V₆O₁₃{(OCH₂)₃C–NH(BOC)}₂]· 2DMA, has been characterized in the solid-state by single-crystal X-ray diffraction and infrared spectroscopy, and in solution by multinuclear (¹H, ¹³C, ¹⁵N and ⁵¹V) and DOSY NMR, and UV–visible spectroscopy.

Graphical Abstract

Keywords:

• Polyoxovanadate
• hybrid
• X-ray structure
• NMR
• diffusion ordered spectroscopy
• BOC

Disclosure statement

No potential conflict of interest was reported by the authors.

Additional information

Funding

Authors gratefully acknowledge financial support from LabEx CHARMMMAT (grant number ANR-11-LBX-0039). This work was also supported by i) University of Versailles Saint Quentin, ii) CNRS, iii) Région Ile de France through DIM Nano K. Ibrahima Fa Bamba thanks the Embassy of Ivory Coast in France for his scholarship. M. Frigoli (ILV) is acknowledged for fruitful discussions.