Preparation of a metal complex
AssigneeJohnson Matthey Public Limited Company
InventorsThomas John Colacot, Gabriela Alexandra Grasa, Hongbo Li
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Abstract
The present invention provides a process for the preparation of a Pd(0)Ln complex, where L is a ligand and n is 2, 3 or 4, comprising the steps of: (a) reacting a Pd(II) complex in at least one solvent with a base and ligand L; and (b) if required, adding further base, optionally in at least one solvent, to form the Pd(0)Ln complex; wherein the at least one solvents in steps a and b are independently the same or different, and provided that when n=2, the Pd(II) complex is not bis[tri(ortho-tolyl)phosphine] palladium chloride. The invention also provides novel Pd(0)L2 and Pd(II) complexes.
Claims29
A process for the preparation of a Pd(0)Ln complex, where L is a ligand and n is 2, comprising the steps of:
- a. reacting a Pd(II) complex in at least one solvent with a base and a ligand L;
- and
- b. if required, adding further base, optionally in at least one solvent, to form the Pd(0)Ln complex;
- wherein the at least one solvents in steps a and b are independently the same or different;
- and
- wherein the Pd(II) complex is selected from the group consisting of Pd(olefin)x(Hal)2, Pd(Hal)2 and M2Pd(Hal)4, in which each Hal is independently a halide, M is a cation, x is 1 or 2, and wherein when x=1 the olefin is a diolefin and when x=2 the olefin is a mono-olefin.
A process for the preparation of a Pd(0)Ln complex, where L is a ligand and n is 3 or 4, comprising the steps of:
- a. reacting a Pd(II) complex in at least one solvent with a base and a ligand L;
- and
- b. if required, adding further base, optionally in at least one solvent, to form the Pd(0)Ln complex;
- wherein the at least one solvents in steps a and b are independently the same or different.
A process for the preparation of a Pd(II) complex of formula 2a or 2b:
- comprising reacting Pd(diolefin) (Hal)2 with (i) hydroxide in water, (ii) an alkoxide in at least one solvent, or (iii) hydroxide in an alcohol ROH, optionally in at least one solvent, in which each Hal is independently a halide, each R is independently H or an optionally substituted C1-15 straight-chain, branched or cyclic alkyl group and the diolefin is cyclooctadiene or norbornadiene.
A process for the preparation of a L2Pd(H)(Hal) complex comprising the steps of:
- a′. optionally preparing a Pd(II) complex of formula 2a or 2b:
- comprising reacting Pd(diolefin)(Hal)2 with (i) hydroxide in water, (ii) an alkoxide in at least one solvent, or (iii) hydroxide in an alcohol ROH, optionally in at least one solvent, wherein each Hal is independently a halide, each R is independently H or an optionally substituted C1-15 straight-chain, branched or cyclic alkyl group and the diolefin is cyclooctadiene or norbornadiene;
- and
- b′. reacting the Pd(II) complex of formula 2a or 2b with ligand L and, if required, at least one solvent, to form the L2Pd(H)(Hal) complex;
- wherein the at least one solvents of steps a′ and b′ are independently the same or different.
A Pd(II) complex of formula 2a:
- wherein each Hal is independently a halide, and each R is independently a substituted C1-15 straight-chain alkyl group, or an optionally substituted C1-15 branched or cyclic alkyl group.
A Pd(II) complex of formula 2b:
- wherein each Hal is independently a halide, and each R is independently H or an optionally substituted C1-15 straight-chain, branched or cyclic alkyl group.
A Pd(0)L2 complex which is [t-Bu2(p-PhMe2N)P]2Pd.
Dependencies are inferred from the claim text.