Synthesis of bis (cyclopentadienyl) and bis (indenyl)...

Details Synthesis of bis (cyclopentadienyl) and bis (indenyl)... Synthesis of bis (cyclopentadienyl) and bis (indenyl)...

2002-06-21

2003-11-04

Nazario-Gonzalez, Porfirio (Department: 1621)

Organic compounds -- part of the class 532-570 series

Organic compounds

Heavy metal containing

C427S252000

Reexamination Certificate

active

06642402

ABSTRACT:

FIELD OF THE INVENTION
This invention relates to bis(cyclopentadienyl) and bis(indenyl) ruthenium complexes which are useful in chemical vapor deposition (CV) and other procedures.
BACKGROUND OF THE INVENTION
The state of the art relevant to this invention as of Jul. 17, 1997 is summarized in U.S. Pat. No. 6,002,036. A process for the synthesis of bis(alkylcyclopentadienyl) ruthenium complexes by treatment of RuCl
3
hydrates and ethylcyclopentadiene or isopropylcyclopentadiene with zinc powder in an alcohol solvent at −30° C. to 0° C. is described.
SUMMARY OF THE INVENTION
The invention comprises synthesis of bis(cyclopentadienyl), bis(alkylcyclopentadienyl), bis(indenyl) or bis(alkylindenyl) liquid and solid ruthenium complexes by treating ruthenium trichloride hydrate and a cyclopentadienyl compound or an indenyl compound with magnesium powder in C
2
to C
8
alkanol, e.g., ethanol. The treating may be accomplished at a temperature from about 10° C. to about −30° C.
DEFINITIONS
As used in this specification, the following terms have the meaning set forth:
(1) Cyclopentadienyl Compound
A compound of the formula
in which each R is independently hydrogen or a C
1
to C
10
alkyl group. C
1
to C
5
monoalkyl cyclopentadienyl compounds are preferred.
(2) Indenyl Compound
A compound of formula
in which each R is independently hydrogen or a C
1
to C
10
alkyl group. C
1
to C
5
monoindenyl compounds are preferred.
DETAILED DESCRIPTION OF THE INVENTION
Ruthenium trichloride dihydrate, a cyclopentadienyl or indenyl compound, and an alkanol, preferably ethanol, are combined and treated with magnesium powder of about minus 100 (−100) to 200 mesh at low temperatures with an appropriate stir out. A bis(cyclopentadienyl) or bis(indenyl) ruthenocene may be isolated by filtration, followed by combination with an aliphatic or aromatic hydrocarbon solvent, preferably hexane or toluene, another filtration, and subsequent passage through a silica column. Final products, if solids, may be isolated in >99% purity in yields of about 65 weight percent by crystallization from a hydrocarbon solvent. High purity liquid products may be isolated by fractional distillation.


REFERENCES:
patent: 6002036 (1999-12-01), Kadokura
patent: 6521772 (2003-02-01), Lienhard et al.
patent: 2002/0058106 (2002-05-01), Okamoto et al.
patent: 2002/0064948 (2002-05-01), Saito et al.
patent: 2002/0065427 (2002-05-01), Okamoto
patent: 2002/0103395 (2002-08-01), Saito

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