Ruthenium Complex Synthesis via Ion Exchange and Extraction

Resolve Bottlenecks,
Find Innovative SolutionsGenerate Solutions

Solution Overview

Problem

Existing methods for synthesizing sodium trans-[tetrachlorobis(1H-indazole)ruthenate (III) are cumbersome due to limited solubility issues, requiring high volumes of solvent and low efficiency.

Innovation Solution

A method involving the reaction of indazolium trans-[tetrachlorobis(1H-indazole)ruthenate (III) with an inorganic alkali metal salt in an aqueous solution, followed by extraction with a water-insoluble organic solvent to produce an alkali metal salt of trans-[tetrachlorobis(1H-indazole)ruthenate (III), optimizing solubility and efficiency.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Quantity of substance

If existing synthesis methods are used for sodium trans-[tetrachlorobis(1H-indazole)ruthenate (III)], then the compound can be produced, but high volumes of solvent are required due to limited solubility

Engineering Contradiction:

Improvesolvent volumeVSAvoidsynthesis process simplicity

Core Design Contradiction:

Quantity of substanceVSEase of manufacture

Solution Approach 1:

The patent changes the solvent system parameters by using a mixture of water and a water-soluble organic solvent (first organic solvent) for the reaction, followed by extraction with a water-insoluble organic solvent (second organic solvent). This parameter change optimizes solubility characteristics and reduces the total volume of solvent required compared to existing methods.

Inventive Principle:

Principle #35Parameter changes

Solution Approach 2:

The patent applies extraction by removing the indazole byproduct from the reaction mixture using a water-insoluble organic solvent. This extraction step separates the desired ruthenium complex from the byproduct, improving purification efficiency while reducing solvent consumption compared to traditional methods.

Inventive Principle:

Principle #2Taking out (Extraction)

2Productivity

If existing synthesis methods are used, then the compound can be produced, but the process efficiency is low

Engineering Contradiction:

Improveprocess efficiencyVSAvoidsynthesis time

Core Design Contradiction:

ProductivityVSLoss of time

Solution Approach 1:

The patent implements a continuous synthesis process where the reaction in aqueous/organic solvent mixture is directly followed by extraction with a second organic solvent. This continuous approach eliminates intermediate isolation steps and maintains productive action throughout, significantly improving process efficiency and reducing overall synthesis time.

Inventive Principle:

Principle #20Continuity of useful action

Solution Approach 2:

The patent utilizes phase transitions by performing the reaction in a water-soluble solvent system and then extracting with a water-insoluble organic solvent. The immiscibility of the two solvent phases creates distinct layers that facilitate easy separation, accelerating the purification process and improving overall productivity.

Inventive Principle:

Principle #36Phase transitions

3Manufacturing precision

If indazolium trans-[tetrachlorobis(1H-indazole)ruthenate (III)] is reacted with inorganic alkali metal salt in aqueous solution, then the desired alkali metal salt product is formed, but indazole byproduct must be removed

Engineering Contradiction:

Improveproduct purityVSAvoidprocess steps

Core Design Contradiction:

Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent uses a water-insoluble organic solvent as an intermediary medium for extraction. This intermediary solvent selectively dissolves the indazole byproduct while leaving the desired alkali metal salt of the ruthenium complex in the aqueous phase, achieving high product purity through a single extraction operation.

Inventive Principle:

Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent segments the reaction mixture into two distinct phases: an aqueous phase containing the desired product and an organic phase containing the indazole byproduct. This segmentation based on solubility differences simplifies the separation process and achieves high manufacturing precision without adding complex purification steps.

Inventive Principle:

Principle #1Segmentation

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 approach provides an efficient and convenient synthesis process with improved yield and reduced solvent usage, enhancing the production of alkali metal salts of trans-[tetrachlorobis(1H-indazole)ruthenate (III) with higher purity and efficiency.

Implementation Method 1

reacting, in an aqueous solution or a mixture of water and a first organic solvent which is water soluble, indazolium trans-[tetrachlorobis(1H-indazole)ruthenate (III)] with an inorganic salt of said alkali metal cation M, to form the compound M-trans-[tetrachlorobis(1H-indazole)ruthenate (III)] and an inorganic salt of indazole

Methodology Applied

Scientific EffectIon exchange: Ion Exchange

Implementation Method 2

extracting said indazole from said M-trans-[tetrachlorobis(1H-indazole)ruthenate (III)] with a second organic solvent which is not substantially water soluble

Methodology Applied

Scientific EffectLiquid-liquid extraction: Liquid-Liquid Extraction

Data Source

PatentUS8362266B2Method of manufacturing a ruthenium complex

Publication Date: 2013.01.29 NIIKI PHARMA ACQUISITION CORP 2

AI summary

A method of making an alkali metal salt of trans-[tetrachlorobis(1H-indazole)ruthenate (III)] is disclosed.