Continuous Flow Production of Boronic Acid Derivatives

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Solution Overview

Problem

Current methods for large-scale production of boronic acid derivatives are hindered by the need for low temperatures, exclusion of water, and precise control of Lewis acid stoichiometry, making them difficult to scale up and resulting in lower yields and higher impurities.

Innovation Solution

A continuous flow process using stainless steel tubular reaction apparatus, where alkyl lithium and dichloromethane are combined to form an intermediate, which is then reacted with a compound in a continuous flow conduit, followed by treatment with a Lewis acid to produce boronic acid derivatives, allowing for higher temperatures and easier scalability.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If batch process with very low temperature (≤ -90 °C) and strict water exclusion is used, then reaction yield is improved, but device complexity and difficulty of operation increase significantly

Engineering Contradiction:
Improvereaction yieldVSAvoiddevice complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent employs a continuous flow process where reactions proceed continuously through controlled segments rather than batch processing. This allows maintenance of low temperatures and water exclusion conditions continuously, achieving high yields while simplifying operational complexity through automated flow control

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The reaction process is divided into discrete segments within the flow system, with each segment performing a specific function (mixing, reaction, separation). This segmentation allows independent optimization of each step while maintaining overall process simplicity and scalability

Inventive Principle:
Principle #1Segmentation

2Manufacturing precision

If batch process with very low temperature (≤ -90 °C) and strict water exclusion is used, then reaction yield is improved, but productivity decreases due to difficult scalability

Engineering Contradiction:
Improvereaction yieldVSAvoidproductivity
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The continuous flow process enables uninterrupted production, eliminating the start-stop nature of batch processing. This continuity directly increases productivity while maintaining the low temperature conditions necessary for high yields, and allows straightforward scaling by increasing flow rates or parallelizing flow channels

Inventive Principle:
Principle #20Continuity of useful action

3Manufacturing precision

If precise control of Lewis acid stoichiometry is required, then product purity is improved, but ease of operation deteriorates

Engineering Contradiction:
Improveproduct purityVSAvoidease of operation
Core Design Contradiction:
Manufacturing precisionVSEase of operation

Solution Approach 1:

The flow system incorporates feedback mechanisms through controlled addition of reagents based on real-time monitoring of reaction progress. This ensures precise Lewis acid stoichiometry is maintained automatically, achieving high product purity while eliminating the need for manual intervention and complex operational procedures

Inventive Principle:
Principle #23Feedback

4Manufacturing precision

If batch process is used, then reaction selectivity can be maintained, but equipment volume required increases for large scale production

Engineering Contradiction:
Improvereaction selectivityVSAvoidequipment volume
Core Design Contradiction:
Manufacturing precisionVSVolume of stationary object

Solution Approach 1:

The patent transitions from three-dimensional batch reactor volumes to a linear flow path geometry. This dimensional change allows large-scale production to be achieved by extending the flow path length or increasing flow rate, rather than requiring proportionally larger reactor volumes, thus maintaining selectivity while reducing equipment footprint

Inventive Principle:
Principle #17Another dimension (Dimensionality change)

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 achieves high yield and selectivity, with successful production of over 880 kg of boronic acid derivatives with an average yield of over 90%, improving reproducibility and reducing equipment volumes needed.

Implementation Method 1

combining the first continuous flow of alkyl lithium and the continuous flow of dichloromethane at an input of a first continuous flow conduit to yield a continuous flow of a first reaction intermediate

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

combining the continuous flow of the first reaction intermediate and the continuous flow of the compound of Formula (IIa) or (IIb) at an input of the second continuous flow conduit to yield a second reaction intermediate

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 3

collecting the second reaction intermediate at the output of the second continuous flow conduit and treating with a Lewis acid to yield the compound of Formula (Ia) or (Ib)

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Data Source

PatentEP3233869B1Apparatus and continuous flow process for production of boronic acid derivatives
Publication Date: 2019.09.25 REMPEX PHARMACEUTICALS INC
  • EP3233869B1 patent drawingFigure 1
  • EP3233869B1 patent drawingFigure 2
  • EP3233869B1 patent drawingFigure 3A

AI summary

A process for a continuous production of a boronic acid derivative based on a Matteson boronic ester homologation and an apparatus of performing the process are disclosed.