Crystalline Intermediates for Macrolide Synthesis

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

The synthesis of macrolides like F152 and its derivatives is hindered by complex and costly chromatographic purification steps, limiting the yield and purity of these biologically active compounds.

Innovation Solution

New methods and intermediates are developed for the preparation of macrolides, which reduce or eliminate the need for chromatographic purification, increasing yield and purity by providing crystalline and highly soluble intermediates that can be isolated without extensive chromatography.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional synthesis methods are used to prepare macrolides, then the biological activity can be achieved, but the synthesis requires complex and costly chromatographic purification steps

Engineering Contradiction:
Improvebiological activityVSAvoidchromatographic purification steps
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent extracts and removes the problematic chromatographic purification steps from the synthesis pathway by designing a route that produces crystalline intermediates可直接纯化。The key is to eliminate the need for complex chromatography by using crystallization-based purification instead.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent changes the physical state parameter of the intermediates from amorphous to crystalline form. This phase change enables simple filtration and washing to achieve high purity, replacing the need for complex chromatographic separation while maintaining biological activity.

Inventive Principle:
Principle #35Parameter changes

2Quantity of substance

If conventional synthesis methods are used to prepare macrolides, then the product can be obtained, but the yield is limited due to multiple purification steps

Engineering Contradiction:
ImproveyieldVSAvoidproduction time
Core Design Contradiction:
Quantity of substanceVSLoss of time

Solution Approach 1:

The patent establishes a continuous synthesis pathway where crystalline intermediates can be directly carried forward to the next reaction step after simple filtration, eliminating time-consuming chromatographic purification steps and maintaining continuous productive action throughout the synthesis.

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The patent performs preliminary crystallization of intermediates during the synthesis pathway, preparing them in advance for the next reaction step. This preliminary purification action eliminates the need for subsequent chromatographic steps, increasing both yield and reducing production time.

Inventive Principle:
Principle #10Preliminary action

3Manufacturing precision

If conventional synthesis methods are used to prepare macrolides, then the product can be synthesized, but extensive chromatographic steps are required to remove impurities

Engineering Contradiction:
ImprovepurityVSAvoidchromatographic purification steps
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The patent utilizes phase transitions from amorphous to crystalline form of intermediates to achieve purification. The crystallization process selectively forms solid crystals that can be easily separated from impurities through filtration, achieving high purity without complex chromatographic equipment.

Inventive Principle:
Principle #36Phase transitions

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

These methods enhance the yield and purity of macrolides, reducing production time and costs while minimizing the use of organic solvents and chromatographic steps, leading to more efficient and cost-effective synthesis.

Implementation Method 1

providing crystalline and highly soluble intermediates that can be isolated without extensive chromatography

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentEP2231634B1Intermediates in the synthesis of zearalenone macrolide analogs
Publication Date: 2016.05.11 EISAI R&D MANAGEMENT CO LTD
  • EP2231634B1 patent drawingFigure 1
  • EP2231634B1 patent drawingFigure 2
  • EP2231634B1 patent drawingFigure 3A~3B

AI summary

Disclosed herein are methods and intermediates useful in the preparation of macrolides, e.g., compounds of formula (IV), wherein R1-R12 are as defined herein.