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Preparation method for nickel dipyrazoborate complex

A technology of dipyrazole borate and nickel complexes, applied in nickel organic compounds, organic chemical methods, chemical instruments and methods, etc., can solve the problems of limited types and applications, and achieve the effect of enriching types

Inactive Publication Date: 2018-10-23
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the current types and applications of such complex catalysts are very limited

Method used

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  • Preparation method for nickel dipyrazoborate complex
  • Preparation method for nickel dipyrazoborate complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] All operations were performed under a high-purity nitrogen atmosphere. In the glove box, add 0.320 g Na[BBN(3,5-Me 2 -pz)] and 0.654 g NiCl 2 (PPh 3 ) 2 , move the schlenk reaction bottle out of the glove box after sealing with a stopper, then add 40 mL of dichloromethane solvent and stir at room temperature for 10 hours, then filter to remove insoluble matter, drain the solvent and add n-hexane long crystals to obtain pure target product Ni[BBN( 3,5-Me 2 -pz) 3 BBN(OH) 2 ], weighing 0.505g, yield 95%.

Embodiment 2

[0017] All operations were performed under a high-purity nitrogen atmosphere. In the glove box, add 0.320 g Na[BBN(3,5-Me 2 -pz)] and 0.654 g NiCl 2 (PPh 3 ) 2 , move the schlenk reaction bottle out of the glove box after sealing with a stopper, then add 40 mL of dichloromethane solvent and stir at room temperature for 11 hours, then filter to remove insoluble matter, drain the solvent and add n-hexane long crystals to obtain pure target product Ni[BBN( 3,5-Me 2 -pz) 3 BBN(OH) 2 ], weighing 0.494g, yield 93%.

Embodiment 3

[0019] All operations were performed under a high-purity nitrogen atmosphere. In the glove box, add 0.320 g Na[BBN(3,5-Me 2 -pz)] and 0.654 g NiCl 2 (PPh 3 ) 2 , move the schlenk reaction bottle out of the glove box after sealing with a stopper, then add 40 mL of dichloromethane solvent and stir at room temperature for 12 hours to remove insoluble matter by filtration, drain the solvent and add n-hexane long crystals to obtain pure target product Ni[BBN( 3,5-Me 2 -pz) 3 BBN(OH) 2 ], weighing 0.500g, yield 94%.

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Abstract

The invention discloses a preparation method for a nickel dipyrazoborate complex. Under an oxygen-free condition, Na[BBN(3,5-Me2-pz)] and NiCl2(PPh3)2 are added into a reaction vessel, dichloromethanesolution is then added, and after 10 to 13 hours of stirring is performed under room temperature, the pure target product Ni[BBN(3,5-Me2-pz)3BBN(OH)2] is prepared. The preparation method is easy to operate, the novel metal dipyrazoborate complex is synthesized, and can be applied to mass production.

Description

technical field [0001] The invention belongs to the technical field of synthesis of nickel complexes, and in particular relates to a preparation method of a dipyrazole borate nickel complex. Background technique [0002] Bipyrazole borate complexes are a very important class of scorpion complexes. Since Trofimenko reported the first case of polypyrazole borate ligands, this type of ligands have been widely used as anionic σ donors for synthesis various complexes. These borate ligands and their complexes have important applications in the fields of coordination chemistry, bioinorganic chemistry, and catalytic chemistry. The dipyrazole borate ligand, due to its adjustable steric and electronic effects, is one of the ideal ligands for studying the relationship between the structure and reactivity of complexes. [0003] By changing the substituent of the pyrazole ring, the steric hindrance of the dipyrazole borate ligand can be changed to control the size and shape of the meta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/04C07F5/02
CPCC07F15/045C07B2200/13C07F5/02
Inventor 赵茜怡窦婷关新婷张絜陈学年
Owner HENAN NORMAL UNIV