Formula I Intermediates for PQQ Synthesis

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Solution Overview

Problem

Current synthetic routes for pyrroloquinoline quinone (PQQ) and related compounds are complex, laborious, and involve numerous steps, making them inefficient and costly for large-scale production.

Innovation Solution

The use of compounds of Formula I, which are synthesized through a simplified process involving specific reactions with esters and bases, reducing the number of steps and improving yield, allowing for the efficient production of PQQ and its salts.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If traditional synthetic routes (Corey et al., Martin et al.) are used for PQQ production, then the synthesis can be completed, but the process involves 9-10 steps with complex and laborious workup procedures

Engineering Contradiction:
Improvesynthesis efficiencyVSAvoidnumber of synthesis steps
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The patent segments the complex 9-10 step synthesis into distinct modular stages: (i) formation of compound of formula I from compounds of formula II and III, (ii) conversion to compound of formula IV, (iii) cyclization to compound of formula V, and (iv) oxidation to final PQQ product. Each stage uses specific reagents and conditions optimized for that transformation, allowing independent optimization and simplification of each step.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The patent performs preliminary actions by pre-forming key intermediates (compounds of formula I) with predetermined structural features that facilitate subsequent transformations. The workup procedures are also designed as preliminary actions that simplify later steps, such as using extraction methods that pre-concentrate the product in a form ready for the next reaction.

Inventive Principle:
Principle #10Preliminary action

2Ease of operation

If traditional synthetic routes are used, then PQQ can be synthesized, but the workup procedure is very complex and laborious

Engineering Contradiction:
Improveworkup procedure simplicityVSAvoidtime for isolation and purification
Core Design Contradiction:
Ease of operationVSLoss of time

Solution Approach 1:

The patent employs disposable extraction systems using common solvents (ethyl acetate, dichloromethane, hexane) that can be easily removed by evaporation. These simple, readily available materials replace complex purification equipment and procedures, making the workup faster and easier while allowing complete removal of solvents to obtain pure product.

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

Solution Approach 2:

The patent changes physical parameters such as solvent polarity, temperature, and pH to control product isolation. For example, adjusting the pH during extraction, using solvents with different polarities for selective extraction, and controlling temperature during crystallization steps enable simple yet effective separation without complex equipment.

Inventive Principle:
Principle #35Parameter changes

3Productivity

If multi-step synthesis is used for PQQ production, then the target compound can be obtained, but the process is costly and inefficient for large-scale production

Engineering Contradiction:
Improvelarge-scale production efficiencyVSAvoidmanufacturing cost
Core Design Contradiction:
ProductivityVSEase of manufacture

Solution Approach 1:

The patent develops a universal synthesis platform where compounds of formula I serve as versatile intermediates that can be converted to multiple different products (PQQ, pyrroloquinoline derivatives, other heterocyclic compounds) through variations of the same core reaction sequence. This multi-functionality allows the same basic methodology to be applied across different target molecules, reducing development costs and improving manufacturing efficiency.

Inventive Principle:
Principle #6Universality (Multi-functionality)

Solution Approach 2:

The patent optimizes reaction parameters (temperature, pressure, catalyst loading, solvent choice, reaction time) for each transformation step to maximize yield and minimize byproducts. By carefully controlling these parameters, the process achieves high efficiency suitable for large-scale production while reducing material waste and energy consumption.

Inventive Principle:
Principle #35Parameter changes

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

The new process results in a cost-effective, environmentally friendly, and efficient synthesis of PQQ and its salts, reducing the number of steps from 10 to 6 and significantly improving yield, making it suitable for large-scale production.

Implementation Method 1

reacting a compound of Formula III with ester and base to obtain the compound of Formula I

Methodology Applied
Scientific EffectNucleophilic substitution: Chemical Bonding

Implementation Method 2

reacting a compound of Formula III with ester and base to obtain the compound of Formula I

Methodology Applied
Scientific EffectCondensation reaction: Chemical Bonding

Implementation Method 3

reacting the compound of Formula I with reducing agent to obtain a compound of Formula IV

Methodology Applied
Scientific EffectReduction: Reduction

Data Source

PatentEP3004047B1Compounds of '3-(5-substituted oxy-2,4-dinitro-phenyl)-2-oxo-propionic acid ester', process and applications thereof
Publication Date: 2017.02.22 ANTHEM BIOSCI PVT
  • EP3004047B1 patent drawingFigure 1~2
  • EP3004047B1 patent drawingFigure 3
  • EP3004047B1 patent drawingFigure 4

AI summary

The present disclosure relates to compounds of Formula (I) and process of obtaining the same. Said compounds of Formula (I) is employed in the syntheses of pyrroloquinoline quinone (PQQ), 4,5-dioxo-4,5-dihydro-1H-pyrrolo[2,3-f]quinoline-2,7,9-tricarboxylic acid 2-allyl ester, 5-ethoxy-5-hydroxy-4-oxo-4,5-dihydro-1H-pyrrolo[2,3-f]quinoline-2,7,9-tricarboxylic acid, 5- hydroxy-6-(1,1,4-trioxo-1 lambda* 6*-1,2, 5 -thiadiazolidin-2-yl)-1H-indole-2-carboxylic acid and its pharmaceutically acceptable salts. Said syntheses of compounds via. compounds of Formula (I) as intermediates employ minimum number of steps resulting in a shorter process and has improved efficiency along with many other advantages.