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Method for the preparation of bis(pentadienyl)-complexes of iron group metals

A technology of coordination compounds and compounds, applied in chemical instruments and methods, metallocenes, organic chemistry, etc., can solve problems such as insufficient decomposition of metal pentadienyl compounds

Active Publication Date: 2011-10-19
HERAEUS PRECIOUS METALS GMBH & CO KG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, the water in the hydrate may not be sufficient to decompose the undesired metal pentadienyl compounds, and these impurities may still be present in the coordination compounds of the prior art

Method used

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  • Method for the preparation of bis(pentadienyl)-complexes of iron group metals
  • Method for the preparation of bis(pentadienyl)-complexes of iron group metals
  • Method for the preparation of bis(pentadienyl)-complexes of iron group metals

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0026] Example: by RuCl 3 Hydrate+HEtCp to prepare bis(EtCp)Ru(II)

[0027] Add 3.5L ethanol, 671g HEtCp (dimer, available from Sigma-Aldrich Company) and 144g aluminum powder (particle size less than 75 microns, Purity 99+%, available from Sigma-Aldrich). In another argon-flushed flask, 415 g of RuCl 3 Hydrate (manufactured by W.C. Heraeus, Santa Fe Springs CA), 625 mL of water, and 1876 mL of ethanol were mixed. The contents of the 12 L flask were cooled to below -20°C (253K) and the ruthenium solution was added slowly and steadily for 3 hours. After all the ruthenium solution was added, the reaction system was slowly warmed to room temperature. After the reaction was completed, the reaction system appeared as a gray slurry.

[0028] The resulting slurry was filtered under inert gas, concentrated to an oily solid, and extracted into hexanes. The hexane extract was concentrated to give an amber oil. Subsequent high vacuum distillation afforded 490 g of the desired prod...

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Abstract

The invention relates to a method for the preparation of bis(pentadienyl)-complexes of iron group metals, especially a method for preparing organometallic complexes of the general formula (I): M(RPD)2 (I) in which M may be iron, ruthenium, or osmium, R is hydrogen or an alkyl group having about 1 to 4 carbon atoms, and PD is a cyclic or open chain dienyl system that is known to form a sandwich type complex is provided. The complexes having formula (I) have a metal purity of at least about 99.99%. The method involves reacting a M(III) trichloride hydrate with an HRPD compound and at least one reducing metal, such as aluminum, in an alcohol solvent.

Description

technical field [0001] The present invention relates to a method for preparing bis(dienyl) complexes of iron group metals (for example, bis(pentadienyl) complexes of iron group metals). Background technique [0002] M (RPD) 2 Type organometallic coordination compounds are usually used in processes related to the formation of thin films, where M represents iron, ruthenium or osmium, R represents hydrogen or an alkyl group, and PD can be a cyclic or open-chain dioxane that forms a sandwich type coordination compound. alkenyl system. For example, thin films of ruthenium can be used in semiconductor manufacturing where resistive or conductive layers are required, such as decorative coatings on ceramics, or in heat-resistant surfaces, such as those in automotive windows. Documents related to electronic components describe the formation of conductive and resistive films by chemical vapor deposition (CVD). For electronic devices, high purity raw materials are essential to achiev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F17/00C07F17/02
CPCC07F17/02
Inventor J·沙普K·金S·杰弗里
Owner HERAEUS PRECIOUS METALS GMBH & CO KG