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Process for preparation of ruthenium complexes

A complex and unsubstituted technology, applied in ruthenium organic compounds, platinum group organic compounds, organic chemistry, etc., can solve problems such as insecurity on an industrial scale

Inactive Publication Date: 2022-01-04
JOHNSON MATTHEY PLC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Furthermore, these methods use organic flammable solvents at reflux, as well as toxic solvents such as benzene and DMF, all of which are unsafe on an industrial scale
Additionally, these methods revealed differences between the ease of addition of three nitrogen-containing heterocyclic bidentate ligands on ruthenium, necessitating a multistep synthetic procedure

Method used

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  • Process for preparation of ruthenium complexes
  • Process for preparation of ruthenium complexes
  • Process for preparation of ruthenium complexes

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0173] Example 1: With EtOH:H 2 The change of O solvent composition, towards [Ru(bpy) 3 ][Cl] 2 conversion rate of

[0174] In EtOH as the sole solvent, the reaction was performed to give only about 5% of the desired product [Ru(bpy) 3 ][Cl] 2 (Example 1A). 10:1 EtOH:H 2 O ratio provided at 11% conversion [Ru(bpy) 3 ][Cl] 2 (Example 1B). Increase the water content first to 2:1, then to 1:2EtOH:H 2 O ratio, obtained to [Ru(bpy) 3 ][Cl] 2 (47% and 97%, respectively; Examples 1C and 1D). EtOH:H 2 A further stepwise change of O to 1:2.5 and 1:3 yielded the desired product at near quantitative conversions [Ru(bpy) 3 ][Cl] 2 , and the isolated yields were 78% and 80%, respectively (Examples 1E and 1F). Reduce the ethanol content even further to 1:10 EtOH:H 2 O ratio, increased the isolated yield to 92% (Example 1G). Complete removal of ethanol from the reaction mixture yields [Ru(bpy) 3 ][Cl] 2 100% conversion and 94% isolated yield (Example 1H). The results ...

Embodiment 2-7

[0180]A 100 mL two-neck round bottom flask equipped with a condenser, nitrogen inlet fitting, and a Teflon-coated stir bar was charged with the Ru precursor and 2,2'-bipyridine. The flask was sealed, then evacuated and backfilled with nitrogen three times. Solvent was added via syringe, and the reaction was stirred at the indicated temperature for 16 hours. The reaction mixture was cooled to ambient temperature, and anti-solvent was added (if applicable). The resulting mixture was stirred for 30 minutes, and the solid was isolated by filtration. The solid was washed with the indicated solvent and dried under vacuum. In some cases, the resulting solids were characterized by NMR spectroscopy and elemental analysis. The results are shown in Table 2.

Embodiment 2

[0181] Embodiment 2: [Ru(Cl) 2 (p-cymene)] 2 (0.61g, 1mmol); 2,2'-bipyridine (0.94g, 6.02mmol); H 2 O (4.5 mL) and THF (0.45 mL), 100 °C, 16 hours; acetone (15 mL) as anti-solvent; acetone (2 x 10 mL) to wash the final product. The title compound was obtained as a bright orange solid (1.27 g, 85%).

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Abstract

A process for the preparation of a complex of formula (I), comprises the step of reacting a complex of formula (II) or a complex of formula RuX3.H2O (IV) with a bidentate ligand of formula (III), wherein R1, R2, R3, R4, R5, R6, R7, R8, R9, R10, A, B, and X are described in the specification; the molar ratio of the complex of formula (II) : the bidentate ligand of formula (III) is about 1 : 6 to about 1 : 8, or the molar ratio of the complex of formula (IV) : the bidentate ligand of formula (III) is about 1 : 3 to about 1 : 4; and the process is carried out in water or a water-based solvent, and the water-based solvent comprises at least 60% water (by volume) and an organic solvent, at one or more temperatures in the range of about 80 DEG C to 110 DEG C.

Description

technical field [0001] The present invention relates to the preparation of homogeneous ruthenium complexes comprising nitrogen-containing heterocyclic bidentate ligands. Background technique [0002] Uniform Ru(bipy) 3 I 2 (bipy=2,2'-bipyridine) by RuCl 3 ·3H 2 A solution of O and 25% excess 2,2-bipyridine (i.e. ratio Ru:NN=1:3.75) in 95% EtOH was heated at reflux for 72 hours before being filtered, evaporated, extracted in benzene, and extracted from the aqueous solution of KI obtained by precipitation in (Palmer et al., Inorg. Chem., 1966, 5(5), 864). [0003] Goss et al. reported by first making RuCl in the presence of LiCl at reflux in DMF 3 ·3H 2 O reacts with phen-diketone at a ratio of Ru:NN=1:2 to produce Ru(phen-diketone) 2 Cl 2 , after which 1.2 equiv of phen-diketone was added at reflux in EtOH / H 2 A solution in a 50 / 50 mixture of O for the synthesis of the homozygous [Ru(phen-diketone) in a step-by-step procedure 3 ](PF 6 ) 2 2H 2 O (phen-diketone = ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/26C07D471/04C07D241/12C07D239/26
CPCC07D213/26C07D471/04C07D241/12C07D239/26C07D213/22C07F15/0053C07D401/04C07D403/04
Inventor D·J·阿诺德T·柯拉科特B·加德纳C·西楚林P·D·坦奇尼
Owner JOHNSON MATTHEY PLC