Propionamide Derivative Crystal Form A Stability

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Solution Overview

Problem

Existing schizophrenia drugs face challenges with adverse reactions and stability issues due to variations in crystalline form, which affect their chemical stability and scalability in production.

Innovation Solution

A specific crystalline form, Crystal Form A, of a propionamide derivative with defined X-ray powder diffraction and Raman spectrum peaks, and a preparation method involving solvent evaporation or precipitation, is developed to enhance stability and purity, allowing for improved clinical application.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Adaptability or versatility

If different crystalline forms are obtained through various preparation methods, then production flexibility is improved, but chemical stability and product reliability deteriorate

Engineering Contradiction:
Improveproduction flexibilityVSAvoidchemical stability
Core Design Contradiction:
Adaptability or versatilityVSReliability

Solution Approach 1:

The patent applies parameter changes by systematically varying preparation conditions (solvent type, temperature, pH, concentration) to identify and isolate the specific set of parameters that produces Crystal Form A with superior chemical stability. This transforms the approach from accepting any crystalline form to precisely controlling formation parameters to achieve the desired stable form.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs feedback mechanisms through characterization techniques (X-ray diffraction, NMR, mass spectrometry) to monitor and verify the crystalline form obtained during preparation. This feedback loop allows real-time adjustment of preparation conditions to ensure consistent formation of Crystal Form A, thereby maintaining chemical stability while enabling reproducible production.

Inventive Principle:
Principle #23Feedback

2Ease of manufacture

If crystalline form structure is not controlled, then preparation process simplicity is maintained, but product stability and manufacturing precision deteriorate

Engineering Contradiction:
Improvepreparation process simplicityVSAvoidcrystalline form purity
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The patent applies preliminary action by pre-establishing optimized preparation conditions before actual production. This includes pre-selecting appropriate solvents, pre-determining optimal temperatures and pH levels, and pre-planning the addition sequence of reagents. These preliminary preparations ensure that when the actual crystallization occurs, Crystal Form A is obtained with high purity without requiring complex real-time control during manufacturing.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent uses intermediary substances such as specific solvents and additives that facilitate the formation of Crystal Form A. These intermediaries act as mediators between the starting materials and the desired crystalline structure, enabling precise control over crystal formation while maintaining relatively simple preparation procedures. The intermediaries guide the molecular assembly process to yield the stable Crystal Form A.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Productivity

If amorphous drug products are produced, then preparation speed is improved, but product stability and reliability deteriorate

Engineering Contradiction:
Improvepreparation speedVSAvoidproduct stability
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The patent utilizes phase transitions in the crystallization process to transform the drug from an amorphous state to a crystalline state. By controlling the phase transition conditions (temperature, solvent removal rate, pH adjustment), the process achieves rapid formation of Crystal Form A that maintains high stability. The controlled phase transition enables both speed and stability, avoiding the trade-off faced by simple evaporation methods that yield amorphous products.

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

The Crystal Form A exhibits high purity and stability, facilitating scalable production and clinical use, with enhanced chemical stability and bioavailability compared to other forms.

Implementation Method 1

removing the solvent in the solution obtained in step 1 by evaporation to give a precipitate

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 2

obtaining a precipitate from the solution obtained in step 1 by precipitation method

Methodology Applied
Scientific EffectPrecipitation: Precipitation

Implementation Method 3

the Crystal Form A has characteristic peaks at 4.46, 11.30, 13.59, 18.17, 21.38, 22.03, 25.89 in the X-ray powder diffraction pattern obtained by Cu-Kα radiation

Methodology Applied
Scientific EffectX-ray diffraction: X-Ray

Implementation Method 4

the Crystal Form A has a Raman spectrum with characteristic peaks at 3065.5±2 cm -1

Methodology Applied
Scientific EffectRaman scattering:

Implementation Method 5

the Crystal Form A has a DSC with melting endothermic peak values selected from the group consisting of 116.4 to 122.0°C

Methodology Applied
Scientific EffectDifferential scanning calorimetry: Calorimetry

Data Source

PatentEP3896071B1Crystalline form of propionamide derivative and preparation method therefor
Publication Date: 2023.11.01 NHWA PHARMA CORPORATION
  • EP3896071B1 patent drawingFigure 1
  • EP3896071B1 patent drawingFigure 2
  • EP3896071B1 patent drawingFigure 3

AI summary

The present invention relates to crystal form A of a propionamide derivative and a preparation method therefor. The crystal form A of the compound of formula (1) obtained in the present invention has good crystalline stability and chemical stability, and can be better used in clinical treatment.