Process for the preparation of bis(pentadienyl)-complexes of iron group metals
View Patent ↗A method for preparing organometallic complexes of the general formula (I): M(RPD) 2 (I) in which M may be iron, ruthenium, or osmium, R is hydrogen or an alkyl group having about 1 to 4 carbon atoms, and PD is a cyclic or open chain dienyl system that is known to form a sandwich type complex is provided. The complexes having formula (I) have a metal purity of at least about 99.99%. The method involves reacting a M(III) trichloride hydrate with an HRPD compound and at least one reducing metal, such as aluminum, in an alcohol solvent.
1. A method of preparing an organometallic complex of formula (I):
M(RPD) 2 (I)
wherein M=iron, ruthenium, or osmium; R=H or an alkyl group having about 1 to 4 carbon atoms; PD=a cyclic or open chain dienyl system that forms a sandwich type complex, and wherein the complex having formula (I) has a metal purity of at least about 99.99%; the method comprising reacting a M(III) trichloride hydrate and an HRPD compound with at least one reducing metal selected from the group consisting of Al, Ga, In, Th, Cd, Hg, Li, Na, Ti, V Cr, Mn, Pb, Ni, Ca, and Cu in an alcohol solvent.
2. The method according to claim 1 , wherein the reducing metal is aluminum.
3. The method according to claim 1 , wherein the reducing metal is in a form of a powder.
4. The method according to claim 1 , wherein at least one M′(RPD) x compound is formed as a byproduct, wherein M′ is a metal other than M and x is an integer determined by a valence of M′, the method further comprising adding to the reaction water in an amount effective to completely decompose the at least one M′(RPD) x compound.
5. The method according to claim 4 , wherein M′ is selecting from the group consisting of Zn, Mg, Fe, and Al.
6. The method according to claim 1 , further comprising purifying the organometallic complex having formula (I) by distilling under reduced pressure.
7. The method according to claim 6 , wherein the distillation is performed with a pot temperature of about 150° C. and a pressure of about 0.2 mmHg.
8. The method according to claim 1 , wherein PD is an optionally substituted non-cyclic or cyclic pentadienyl ligand.
9. The method according to claim 8 , wherein PD is a non-cyclic or cyclic pentadienyl having from about one to about five side chains.
10. The method according to claim 1 , wherein PD is ethylcyclopentadienyl or 2,4-dimethylpentadienyl.
11. The method according to claim 1 , wherein the organometallic complex having formula (I) is bis(ethylcyclopentadienyl)ruthenium(II):
12. The method according to claim 1 , wherein the organometallic complex having formula (I) is bis(2,4-dimethylpentadienyl)ruthenium(II):