| US 7,589,224 B2 | ||
| Method for producing iridium(III) keto ketonates | ||
| Philipp Stoessel, Frankfurt Am Main (Germany); Ingrid Bach, Hofheim (Germany); Amir Parham, Frankfurt (Germany); Esther Breuning, Niedernhausen (Germany); and Hubert Spreitzer, Viernheim (Germany) | ||
| Assigned to Merck Patent GmbH, Darmstadt (Germany) | ||
| Appl. No. 11/659,898 PCT Filed Aug. 10, 2005, PCT No. PCT/EP2005/008670 § 371(c)(1), (2), (4) Date Sep. 20, 2007, PCT Pub. No. WO2006/018202, PCT Pub. Date Feb. 23, 2006. |
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| Claims priority of application No. 04019137 (EP), filed on Aug. 12, 2004. | ||
| Prior Publication US 2008/0132720 A1, Jun. 05, 2008 | ||
| Int. Cl. C07F 15/00 (2006.01) | ||
| U.S. Cl. 556—136 | 32 Claims |
| 1. A process for the preparation of iridium(III) complexes containing structural units of formula (1)
[LnIrXaYa]x Formula (1)
wherein
X and Y are, identically or differently on each occurrence, a monodentate, monoanionic ligand which is bonded to the iridium
via a heteroatom;
n is on each occurrence 2 or 3;
a is 0 if n is 3 and is 1 if n is 2;
x is −1 when n is 2 and a is 1 and x is 0 when n is 3 and a is 0;
L is on each occurrence, identically or differently, a ligand of formula (2) which coordinates to Ir via both oxygen atoms
![]() wherein
R1 and R2 are, identically or differently on each occurrence, H, CN, a straight-chain, branched or cyclic alkyl group having up to 20
C atoms, or a straight-chain, branched or cyclic alkoxy group having up to 20 C atoms, wherein one or more non-adjacent CH2 groups of said alkyl or alkoxy groups are optionally replaced by —O—, —S—, —NR3—, —CONR3—, —CO—O—, —CR3═CR3— or —C≡C— and wherein one or more H atoms may be replaced by F, or an aromatic or heteroaromatic ring system having 4 to
14 C atoms, wherein said aromatic or heteroaromatic ring systems may be substituted by one or more non-aromatic radicals R1; and wherein a plurality of substituents R1 and/or R2 together optionally define a monocyclic or polycyclic aliphatic ring system or a monocyclic or polycyclic aromatic ring system;
and
R3 is, identically or differently on each occurrence, H or an aliphatic or aromatic hydrocarbon radical having up to 20 C atoms,
comprising the steps of
(1) reacting an iridium(III) salt starting compound with compounds containing anions of the formula (2) in a first solvent
or solvent mixture,
(2) partially or fully exchanging the first solvent or solvent mixture with a second solvent or solvent mixture, which is
different from the first solvent or solvent mixture, while substantially retaining the amount of the salt-like components
of the reaction mixture, and
(3) completing the reaction in said second solvent or solvent mixture.
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