Process for producing a biphenyl metallocene complex

1 . A process comprising the steps, in this order:

a) providing a precursor mixture comprising (i) a biphenyl compound of formula (2)

wherein, R 1 , R 2 , R 3 , and R 4 are each independently selected from hydrogen, a halide, an alkyl group having one to twenty carbon atoms, an alkenyl group having one to twenty carbon atoms, an aryl group having one to twenty carbon atoms, an alkoxycarbonyl group having one to twenty carbon atoms, or an alkylaryl group having one to twenty carbon atoms; an alkylsulphide group having one to twenty carbon atoms, an alkoxy group having one to twenty carbon atoms, or an amine group; and wherein Z 1 is hydrogen; and (ii) a tertiary amine compound;

and

b) adding at a temperature between 18° C. to 65° C., an alkyl and/or aryl lithium compound having one to ten carbon atoms, to the precursor mixture and forming a first lithiated reaction product;

and

c) contacting the first lithiated reaction product with a boronate ester compound of formula (3)

B(OR 11 ) 3   (3)

and obtaining a boronate reaction product; wherein R 11 is independently selected from hydrogen, an alkyl group having one to twenty carbon atoms, an alkenyl group having one to twenty carbon atoms, an aryl group having one to twenty carbon atoms, an alkoxycarbonyl group having one to twenty carbon atoms, or an alkylaryl group having one to twenty carbon atoms;

and

d) hydrolyzing the boronate reaction product and forming the boronic anhydride compound of formula (1)

wherein R 1 , R 2 , R 3 , and R 4 are each independently selected from hydrogen, a halide, an alkyl group having one to twenty carbon atoms, an alkenyl group having one to twenty carbon atoms, an aryl group having one to twenty carbon atoms, or an alkylaryl group having one to twenty carbon atoms; an alkylsulphide group having one to twenty carbon atoms, an alkoxy group having one to twenty carbon atoms, or an amine group; and ‘B’ stands for the element boron;

and

e) reacting the boronic anhydride compound of formula (1) with a 2-bromo indenyl of formula (6)

wherein R 5 , R 6 , R 7 , R 8 , R 9 and R 10 are each independently selected from hydrogen, a halide, an alkyl group having one to twenty carbon atoms, an alkenyl group having one to twenty carbon atoms, an aryl group having one to twenty carbon atoms, or an alkylaryl group having one to twenty carbon atoms; an alkylsulphide group having one to twenty carbon atoms, an alkoxy group having one to twenty carbon atoms, or an amine group,

in the presence of a palladium catalyst and forming a metallocene complex precursor of formula (7),

wherein, R 1 to R 10 are as defined herein;

and

f) reacting the metallocene complex precursor of formula (7) with the alkyl and/or aryl lithium compound having one to ten carbon atoms, and forming a second lithiated reaction product;

and

g) reacting for a time period ranging from 4 to 10 hours, the second lithiated reaction product with a transition metal compound of formula (8),

MQ p   (8)

wherein, ‘M’ is a transition metal element selected from Group 3, 4, or 5 of the Periodic System of Elements, ‘Q’ is an halide anion, and ‘P’ is the valency of the transition metal element ‘M’ and indicates the number of halide anion present, and forming a reaction mixture comprising a metallocene complex of formula (4),

wherein, R 1 to R 10 , ‘M’, ‘Q’ and ‘P’ are as defined herein;

and

h) purifying the reaction mixture comprising the metallocene complex of formula (4), by solvent extraction and filtration, and obtaining (i) a purified metallocene ligand of formula (4a),

wherein, R 1 to R 10 , ‘M’, ‘Q’ and ‘P’ are as defined herein,

and (ii) a product effluent comprising a mixture of metallocene complex of formula 4a, metallocene complex precursor of formula 7, partially complexed metallocene complex, and lithium based inorganic salts.

2 . The process according to claim 1 , wherein the tertiary amine compound is tetramethylethylene diamine (TMEDA).

3 . The process according to claim 1 , wherein the alkyl and/or aryl lithium compound is butyl lithium.

4 . The process according to claim 1 , wherein the tertiary amine compound is a bidentate tertiary amine.

5 . The process according to claim 1 , wherein the transition metal element ‘M’ is selected from zirconium, hafnium, or titanium.

6 . The process according to claim 1 , wherein the transition metal element ‘M’ is zirconium.

7 . The process according to claim 1 , wherein the transition metal compound of formula (8) is zirconium tetrachloride (ZrCl 4 ).

8 . The process according to claim 1 , wherein the alkyl and/or aryl lithium compound is selected from methyl lithium, butyl lithium, or phenyl lithium.

9 . The process according to claim 1 , comprising adding at a temperature between 21° C. to 45° C., the alkyl and/or aryl lithium compound having one to ten carbon atoms, to the precursor mixture and forming the first lithiated reaction product.

10 . The process according to claim 1 , comprising adding at a temperature between 25° C. to 35° C., the alkyl and/or aryl lithium compound having one to ten carbon atoms, to the precursor mixture and forming the first lithiated reaction product.

11 . The process according to claim 1 , wherein forming the boronic anhydride compound of formula (1) is conducted at 20° C.-25° C.