Conversion of cyclopentadienyl silyl amines to...

Organic compounds -- part of the class 532-570 series – Organic compounds – Heavy metal containing

Reexamination Certificate

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C556S007000, C556S012000, C556S022000, C556S028000, C556S053000, C502S103000, C526S160000, C526S943000

Reexamination Certificate

active

06590114

ABSTRACT:

FIELD OF THE INVENTION
This invention relates to titanium organometallic complexes which comprise a titanium bisalkoxy moiety or a titanium dichloride moiety.
BACKGROUND OF THE INVENTION
U.S. Pat. Nos. 5,491,246 and 5,504,223 describe the treatment of Me
4
C
5
SiMe
2
N
t
-bu[MgCl]
2
(DME)
n
with titanium tetraisopropoxide to provide Me
4
C
5
SiMe
2
N
t
BuTi(OiPr)
2
which may be treated with SiCl
4
to yield the corresponding dichloride.
DEFINITIONS
In this specification, the following expressions have the meanings set forth hereinafter:
(1) Cyclopentadienyl means any substituted or unsubstituted cyclopentadienyl compound, group or moiety, including but not limited to any alkylcyclopentadienyl, any indenyl, or any alkyl indenyl compound, group or moiety having one or more C
1
to C
10
alkyl ring substituents.
(2) Alkoxide means any radical or group having the formula —OR, wherein R is an alkyl group.
(3) Cyclopentadienyl silyl amine means a compound of Formula
in which Z is a cyclopentadienyl group or moiety and each of R
1
, R
2
and R
3
is independently, the same or a different alkyl group, preferably a C
1
to C
10
alkyl group.
SUMMARY OF THE INVENTION
Pursuant to this invention, an alkali metallide of a cyclopentadienyl silyl amine is reacted with a titanium tetraalkoxide Ti(OR)
4
in which R is a C
1
to C
10
alkyl group, preferably an isopropyl group. The reaction mixture contains the desired bisalkoxide and, as a by-product, an alkali metal alkoxide which may be isolated or converted in situ to an insoluble alkali metal halide to facilitate removal by filtration. The filtrate contains the desired bisalkoxide which may be converted to the corresponding dichloride by treatment with a halogenating agent, e.g., SiCl
4
.
DESCRIPTION OF THE INVENTION
The treatment of a silyl amine with Ti(OR)
4
may be accomplished in any solvent or medium in which the desired titanium bisalkoxide is soluble. Preferred solvents or media are about 10% to 25% by weight mixtures of ethyl ether and a C
6
to C
8
hydrocarbon. The treatment may be accomplished at a temperature of from about −20° to −10° C. The conversion of the alkali metal alkoxide by-product to an alkali metal halide insoluble in the solvent contained in the titanium bisalkoxide synthesis reaction mixture is appropriately conducted at a temperature of from about −35° to −20° C. Conversion of the bisalkoxide to the corresponding dichloride may be accomplished in situ in the synthesis reaction mixture at a temperature of −20° C. to room temperature or refluxing temperature. Useful halogenating agents include SiCl
4
, BCl
3
, and AlCl
3
.


REFERENCES:
patent: 5491246 (1996-02-01), Rosen et al.
patent: 5504223 (1996-04-01), Rosen et al.
patent: 5703257 (1997-12-01), Rosen et al.

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