Ruthenium Complex One-Step Synthesis via Carboxylate Salt
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Solution Overview
Problem
The existing methods for preparing ruthenium carboxylate complexes, such as [Ru(diene)(OOCR)2], are inefficient due to the need for indirect multi-step syntheses, instability of intermediates, low yields, and difficulty in handling, which complicates industrial implementation and catalyst production.
Innovation Solution
A direct one-step process to obtain [(diene)Ru(OOCR)2] complexes from [Ru(diene)Cl2] by reacting with a carboxylic acid salt in a polar aprotic solvent under inert conditions, allowing for the production of stable and efficient catalyst precursors.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Ease of manufacture
If indirect multi-step synthesis is used to prepare ruthenium carboxylate complexes, then the complexes can be obtained, but the synthesis process becomes complex with low yield and difficult handling
Solution Approach 1:
The patent combines multiple synthesis steps into a single direct reaction. The carboxylate complex is prepared in one step by reacting [(diene)RuCl2] with carboxylic acid and base simultaneously, eliminating the need for separate intermediate formation and ligand displacement steps that were required in prior art methods.
Solution Approach 2:
The reaction is segmented into distinct functional components that can be added in a controlled sequence within a single reaction vessel. The carboxylic acid and base are introduced separately to control the reaction pathway, allowing direct formation of the carboxylate complex without forming unstable intermediate species.
2Reliability
If indirect synthesis with intermediate compounds is used, then ruthenium carboxylate complexes can be prepared, but the intermediates are unstable and difficult to handle
Solution Approach 1:
The patent extracts or eliminates the unstable intermediate compounds from the synthesis pathway. By using a direct one-step method where carboxylic acid reacts with the ruthenium precursor in the presence of base, the reaction bypasses the formation of unstable allyl intermediates that require special handling and storage conditions.
Solution Approach 2:
The base acts as an intermediary that facilitates the direct conversion of the ruthenium chloride precursor to the carboxylate complex. The base neutralizes the HCl produced during the reaction, driving the equilibrium toward the desired product without requiring the formation of unstable organic intermediates.
3Productivity
If multi-step synthesis is employed, then ruthenium complexes can be obtained, but the overall yield is low
Solution Approach 1:
The patent implements a continuous one-step synthesis process where the conversion of [(diene)RuCl2] to the carboxylate complex occurs without interruption or isolation of intermediates. The reaction proceeds continuously from starting materials to final product in a single reaction vessel, maximizing material utilization and minimizing losses associated with multiple workup and purification steps.
4Stability of the object's composition
If known synthesis methods are used, then ruthenium carboxylate complexes can be prepared, but inert atmospheres are required for handling and storage
Solution Approach 1:
The patent changes the chemical parameters of the synthesis process by using a direct reaction pathway that produces thermodynamically stable carboxylate complexes. The resulting complexes have enhanced stability due to the strong Ru-O carboxylate bonds formed in the direct synthesis, eliminating the need for inert atmosphere protection during handling and storage.
Applied Scientific Principles
This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.
Function Achieved in This Case
This process simplifies the synthesis, increases yield, and produces stable ruthenium complexes suitable for catalyst production, enabling efficient preparation of [Ru(PP)(OOCR)2] catalysts without the need for inert atmospheres during handling and storage.
Implementation Method 1
Some ruthenium carboxylates complexes of general formula [Ru(diene)(OOCR) 2 ] n , with n equals 1 or 2, have been described as useful starting compounds for the preparation of a number of Ruthenium-diphosphine (PP) complexes of formula [Ru(PP)(OOCR) 2 ], which are good catalysts, for example, in the hydrogenation of carbon-carbon double bonds
Data Source
AI summary
The present invention relates to the field of one step process for the preparation of monomeric or dimeric [Ru(diene)(OOCR)2]n complexes from [(diene)RuCl2]n, as well as a new class of [Ru(diene)(OOCR)2]n complexes and their use to prepare [Ru(PP)(OOCR)2] complexes, which are good catalysts.