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US5474716A
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Process for the preparation of bridged cyclopentadienylmagnesium compounds and use thereof for preparing metallocenes
Assignee: Chemtura Organometallics GmbH
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Filing: 1995-02-22
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Granted: 1995-12-12
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Expires: 2015-02-22
Abstract
Abstract Disclosed are processes for the preparation of new bridged cyclopentadienylmagnesium compounds of the general formula Q(CpR a )(Cp'R' a ')Mg, and the use thereof for preparing bridged metallocenes.
Inventors
- 👤 Richard Lisowsky
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 02:32
CPC Classifications
C; C07; C07F; C07F17/00; C07F17/02; C07F3/00; C07F3/02; C07F7/00; C07F7/02; C07F7/08; C07F7/0803; C07F7/0825; C07F7/0827
Claims Analysis
Total Claims: 9
Claim 1
Independent Claim
233 words
A process for preparing a compound of the general formula (1) Q(CpR.sub.a)(Cp'R'.sub.a ')Mg (1) wherein Cp is a cyclopentadienyl or an indenyl radical; R and R' are the same or different and each is selected from the group consisting of alkyl, phosphine, amino, alkylamino, dialkylamino, alkoxy, alkoxy-alkyl, aryl-alkyl, and aryloxy-alkyl groups; 0≦a≦4 and 0≦a'≦4; Cp' is cyclopentadienyl or indenyl, or when a' is 1, Cp'R' can be NR" wherein R" is a C 1 -C 12 alkyl or a C 6 -C 10 aryl radical; and Q is a single-membered or multi-membered bridge between Cp and Cp' and represents (R.sup.1 --Z--R.sup.2).sub.b, wherein R 1 and R 2 are identical or different and each is a hydrogen atom, a C 1 -C 10 alkyl group or a C 6 -C 10 -aryl group; Z is carbon, silicon or germanium; and b is 1, 2 or 3; said process comprising reacting a bridged cyclopentadienyl compound of the general formula Q(CpR a )(Cp'R' a ') in an inert solvent with one or more magnesium compounds of the formula (R 3 R 4 ) c Mg, wherein R 3 and R 4 are each bonded to the Mg and each is independently of one another H or a C 1 -C 12 -alkyl radical and c is 0 or 1, under conditions effective to form a solution of said compound of formula (1) in said inert solvent.
Claim 2
Dependent Claim
233 words
A process for preparing a compound of the general formula (1) Q(CpR.sub.a)(Cp'R'.sub.a ')Mg (1) wherein Cp is a cyclopentadienyl or an indenyl radical; R and R' are the same or different and each is selected from the group consisting of alkyl, phosphine, amino, alkylamino, dialkylamino, alkoxy, alkoxy-alkyl, aryl-alkyl, and aryloxy-alkyl groups; 0≦a≦4 and 0≦a'≦4; Cp' is cyclopentadienyl or indenyl, or when a' is 1, Cp'R' can be NR" wherein R" is a C 1 -C 12 alkyl or a C 6 -C 10 aryl radical; and Q is a single-membered or multi-membered bridge between Cp and Cp' and represents (R.sup.1 --Z--R.sup.2).sub.b, wherein R 1 and R 2 are identical or different and each is a hydrogen atom, a C 1 -C 10 alkyl group or a C 6 -C 10 -aryl group; Z is carbon, silicon or germanium; and b is 1, 2 or 3; said process comprising reacting a bridged cyclopentadienyl compound of the general formula Q(CpR a )(Cp'R' a ') in an inert solvent with one or more magnesium compounds of the formula (R 3 R 4 ) c Mg, wherein R 3 and R 4 are each bonded to the Mg and each is independently of one another H or a C 1 -C 12 -alkyl radical and c is 0 or 1, under conditions effective to form a solution of said compound of formula (1) in said inert solvent.
Claim 3
Dependent Claim
26 words
A process according to claim 1, characterized in that said inert solvent is selected from the group consisting of petroleum ether, heptane, octane, toluene, and xylene.
Claim 4
Dependent Claim
75 words
A process according to claim 1, wherein said one or more magnesium compounds are selected from the group consisting of compounds of the formula (R 3 R 4 ) c Mg in which c is 1 and R 3 and R 4 are identical or different and each is C 2 H 5 --, C 4 H 9 --, C 6 H 13 -- or C 8 H 17 --, and mixtures of said compounds.
Claim 5
Dependent Claim
44 words
A process according to claim 3, characterized in that in the formula (R 3 R 4 ) c Mg, R 3 and R 4 are each octyl or butyl and the ratio of said butyl to octyl substituents is 3:1, and c is 1.
Claim 6
Dependent Claim
85 words
A process according to claim 1 further comprising directly metering said solution of said compound of formula (1) into a solution of transition metal halide of the formula M(X) m wherein M is Sc, Ti, Zr, Hf or Fe, X is Cl or Br, and m is the oxidation state of M, in an ether or aromatic hydrocarbon solvent in stoichiometric amounts at a temperature effective to form a compound of the formula Q(CpR a )(Cp'R' a ')M(X) n wherein n is m minus 2.
Claim 7
Dependent Claim
218 words
A process for preparing a compound of the general formula (2) Q(CpR.sub.a)(Cp'R'.sub.a)M(X).sub.n ( 2) wherein Cp is a cyclopentadienyl or an indenyl radical; R and R' are the same or different and each is selected from the group consisting of alkyl, phosphine, amino, alkylamino, dialkylamino, alkoxy, alkoxy-alkyl, aryl-alkyl, and aryloxy-alkyl groups; 0≦a≦4 and 0≦a'≦4; Cp' is cyclopentadienyl or indenyl, or when a' is 1, Cp'R' can be NR" wherein R" is a C 1 -C 12 alkyl or a C 6 -C 10 aryl radical; and Q is a single-membered or multi-membered bridge between Cp and Cp' and represents (R.sup.1 --Z--R.sup.2).sub.b, wherein R 1 and R 2 are identical or different and each is a hydrogen atom, a C 1 -C 10 -alkyl group or a C 6 -C 10 -aryl group; Z is carbon, silicon or germanium; and b is 1, 2 or 3; X is Cl or Br; M is Sc, Ti, Zr, Hf or Fe; and n is equal to the oxidation state of M in said compound reduced by 2; comprising reacting a compound of the formula Q(CpR a )(Cp'R' a ')Mg with a transition metal halide of the formula M(X) m wherein m is the numerical value of the oxidation state of M, under conditions effective to form said compound of formula (2).
Claim 8
Dependent Claim
218 words
A process for preparing a compound of the general formula (2) Q(CpR.sub.a)(Cp'R'.sub.a)M(X).sub.n ( 2) wherein Cp is a cyclopentadienyl or an indenyl radical; R and R' are the same or different and each is selected from the group consisting of alkyl, phosphine, amino, alkylamino, dialkylamino, alkoxy, alkoxy-alkyl, aryl-alkyl, and aryloxy-alkyl groups; 0≦a≦4 and 0≦a'≦4; Cp' is cyclopentadienyl or indenyl, or when a' is 1, Cp'R' can be NR" wherein R" is a C 1 -C 12 alkyl or a C 6 -C 10 aryl radical; and Q is a single-membered or multi-membered bridge between Cp and Cp' and represents (R.sup.1 --Z--R.sup.2).sub.b, wherein R 1 and R 2 are identical or different and each is a hydrogen atom, a C 1 -C 10 -alkyl group or a C 6 -C 10 -aryl group; Z is carbon, silicon or germanium; and b is 1, 2 or 3; X is Cl or Br; M is Sc, Ti, Zr, Hf or Fe; and n is equal to the oxidation state of M in said compound reduced by 2; comprising reacting a compound of the formula Q(CpR a )(Cp'R' a ')Mg with a transition metal halide of the formula M(X) m wherein m is the numerical value of the oxidation state of M, under conditions effective to form said compound of formula (2).
Claim 9
Dependent Claim
12 words
A process according to claim 6 wherein Cp'R' a ' is NR".
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