Method for preparing cyclopentadienyl-type ligands and metallocene compounds

A process for preparing a metallocene compound comprising:

• (1) reacting an alkali metal salt of a cyclopentadienyl-type compound and an aminofulvene compound to form a monoanion,
• wherein said cyclopentadienyl-type compound is selected from the group consisting of unsubstituted cyclopentadiene, substituted cyclopentadiene, unsubstituted indene, substituted indene, unsubstituted fluorene, and substituted fluorene, wherein the substituents are selected from the group consisting of hydrocarbyl groups containing 1 to 12 carbon atoms, alkoxy groups containing 1 to 12 carbon atoms, and halide,
• wherein said aminofulvene compound is represented by the formula ##STR4## wherein R is an alkyl group containing 1 to 20 carbon atoms or hydrogen, wherein each R' is individually selected from alkyl groups containing 1 to 20 carbon atoms, and each R" is individually selected from the group consisting of hydrocarbyl groups containing 1 to 20 carbon atoms, and n is 0 to 4;
• (2) reacting said monoanion and a reducing agent to form a dianion,
• wherein said reducing agent is selected from the group consisting of alkali metal compounds containing a hydrocarbyl group containing 1 to 20 carbon atoms and hydrogen;
• and
• (3) reacting said dianion and a transition metal-containing compound to form said metallocene compound,
• wherein said transition-metal containing compound is represented by the formula MX.sub.x, wherein M is a Group IVB or VB transition metal, x is the valence of the transition metal, and each X is individually selected from the group consisting of hydrocarbyl groups containing 1 to 12 carbon atoms, alkoxy groups containing 1 to 12 carbon atoms, aryloxy groups containing 6 to 12 carbon atoms, halide and hydrogen.

A process for preparing a cyclopentadienyl-type ligand said process consisting essentially of:

• (1) reacting an alkali metal salt of a cyclopentadienyl-type compound and an aminofulvene compound to form a monoanion,
• wherein said cyclopentadienyl-type compound is selected from the group consisting of unsubstituted cyclopentadiene, substituted cyclopentadiene, unsubstituted indene, substituted indene, unsubstituted fluorene, and substituted fluorene, wherein the substituents are selected from the group consisting of hydrocarbyl groups containing 1 to 12 carbon atoms, alkoxy groups containing 1 to 12 carbon atoms, and halide,
• wherein said aminofulvene compound is represented by the formula ##STR5## wherein R is an alkyl group containing 1 to 20 carbon atoms or hydrogen, wherein each R' is individually selected from alkyl groups containing 1 to 20 carbon atoms, and each R" is individually selected from the group consisting of hydrocarbyl groups containing 1 to 20 carbon atoms, and n is 0 to 4;
• (2) reacting said monoanion and a reducing agent to form a dianion,
• wherein said reducing agent is selected from the group consisting of alkali metal compounds containing a hydrocarbyl group containing 1 to 20 carbon atoms, lithium aluminum hydride, and hydrogen;
• and
• (3) reacting said dianion and water to produce said cyclopentadienyl-type ligand.

A process for preparing a metallocene compound said process consisting essentially of:

• (1) reacting an alkali metal salt of a cyclopentadienyl-type compound and an aminofulvene compound to form a monoanion,
• wherein said cyclopentadienyl-type compound is selected from the group consisting of unsubstituted cyclopentadiene, substituted cyclopentadiene, unsubstituted indene, substituted indene, unsubstituted fluorene, and substituted fluorene, wherein the substituents are selected from the group consisting of hydrocarbyl groups containing 1 to 12 carbon atoms, alkoxy groups containing 1 to 12 carbon atoms, and halide,
• wherein said aminofulvene compound is represented by the formula ##STR6## wherein R is an alkyl group containing 1 to 20 carbon atoms or hydrogen, wherein each R' is individually selected from alkyl groups containing 1 to 20 carbon atoms, and each R" is individually selected from the group consisting of hydrocarbyl groups containing 1 to 20 carbon atoms, and n is 0 to 4;
• (2) reacting said monoanion and a reducing agent to form a dianion,
• wherein said reducing agent is selected from the group consisting of alkali metal compounds containing a hydrocarbyl group containing 1 to 20 carbon atoms and hydrogen;
• and
• (3) reacting said dianion and a transition metal-containing compound to form said metallocene compound,
• wherein said transition-metal containing compound is represented by the formula MX.sub.x, wherein M is a Group IVB or VB transition metal, x is the valence of the transition metal, and each X is individually selected from the group consisting of hydrocarbyl groups containing 1 to 12 carbon atoms, alkoxy groups containing 1 to 12 carbon atoms, aryloxy groups containing 6 to 12 carbon atoms, halide and hydrogen.