Method for synthesizing diphosphine monoxide ligand

Abstract

The invention discloses a method for synthesizing diphosphorus monoxide complex, which is synthesized by using tert-butyl propyl carbonate through the following steps that: 1) in the presence of a catalyst of hetero-atom containing organic alkali, tert-butyl propyl carbonate and a phosphine oxide undergo a condensation reaction in an organic solvent, and then a reaction mixture is extracted by methylene dichloride to form a monophosphine oxide synthon; and 2) under the action of an alkaline material, the monophosphine oxide synthon and disubstituted phosphor undergo a hydrogenation reaction, and a reaction mixture is extracted by methylene dichloride to form the diphosphorus monoxide complex. The method has the advantages that: the synthesis method is simple, economic and practical, and can effectively synthesize the diphosphorus monoxide and overcome the drawbacks of undesirable selectivity and low yield; the synthesized diphosphorus monoxide complex is provided with functional groups such as an ester group with respect to spatial connection groups, belongs to a multifunctional diphosphorus monoxide complex, provides conditions for the expansion of the application range of the complexes, and is particularly applied in the fields of catalysis of solid-carried catalysts, nuclear pharmaceuticals and the like.

Description

【Technical field】 [0001] The invention belongs to the technical field of chemical catalysis, and in particular relates to a synthesis method of a bisphosphine monooxide ligand. 【Background technique】 [0002] Has the following structural general formula R 1 R 2 P-Y-P(O)R 3 R 4 The bisphosphine monooxide (BPMO) ligand (Y is a space group connected by a double bond) is a class of organophosphorus ligands that have a wide range of uses in fields such as chemical catalysis and drug research [V.V.Grushin, Chem.Rev. 2004, 104, 1629-1662.]. From the structural point of view, this kind of ligand has both soft (P) and hard (O) Lewis base coordination atoms. The transition metals form chemically more active metal complexes. These metal complexes can efficiently catalyze a variety of chemical transformations. For example, the complexes formed by rhodium (Rh) and palladium (Pd) with BPMO ligands have shown superior catalytic activity and chemoselectivity in the carbonylation of m...

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Problems solved by technology

[0003] At present, the synthesis methods of bisphosphine monooxide ligands are divided into two categories: one is to couple two monophosphine components with different oxidation states through chemical transformation to produce them. Due to the coupling step It is based on the special chemical reaction of monophosphine components, so this kind of synthesis method is only suitable for the preparation of bisphosphine monooxide ligands with limited structure types. At present, it is mainly used for the connection between diphosphine atoms via 1 to 2 atoms. The synthesis of the bisphosphine monooxide; the other is the preparation of the bisphosphine monooxide ligand by selectively oxidizing one of the tertiary phosphine atoms. The biggest feature of this method is that it is direct, simple, It has a wide range of applications and can be used for the synthesis of bisphosphine monooxide ligands with different lengths of linking groups. In the starting material bisphosphine compounds, each tertiary phosphine unit is quite close in chemical properties, and one of the units is Oxidation does not significantly change the chemical properties of another phosphorus-containing unit, so this oxidation step lacks real selectivity, and the actual reaction process often leads to the formation of multiple products, resulting in low yield and selectivity, and by This creates difficulties in product separation

Although some new oxidation methods have appeared recently, the selectivity problem that plagues such methods has not been solved

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