5-Amino-2,3-Dihydrophthalazine-1,4-Dione Sodium Salt Form III Crystallization

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Solution Overview

Problem

Current pharmaceutical production faces challenges with maintaining the phase purity and bulk density of 5-amino-2,3-dihydrophthalazine-1,4-dione sodium salt, leading to issues in storage stability and biological effectiveness due to polymorphic forms and solubility variations, which can result in inconsistent drug performance and side effects.

Innovation Solution

A new anhydrate form (Form III) of 5-amino-2,3-dihydrophthalazine-1,4-dione sodium salt is developed, characterized by specific X-ray powder diffraction patterns and produced through a process involving dissolution in DMSO followed by evaporation, offering improved bulk density and storage stability without the use of heavy metal catalysts.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional manufacturing processes are used for 5-amino-2,3-dihydrophthalazine-1,4-dione sodium salt, then production can proceed with existing methods, but phase purity and bulk density cannot be maintained, leading to storage stability issues and inconsistent biological effectiveness

Engineering Contradiction:
Improvephase purityVSAvoidmanufacturing process complexity
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

The patent applies parameter changes by modifying the manufacturing process parameters, specifically using DMSO as a solvent and controlling evaporation conditions to transform the crystalline structure from mixed polymorphic forms to pure Form III. This parameter change (solvent type and evaporation control) directly resolves the contradiction by achieving consistent phase purity without requiring overly complex additional processing steps

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent utilizes phase transitions by controlling the transformation from dissolved state through evaporation to crystalline Form III. The controlled evaporation process induces a specific phase transition that yields the desired crystalline form with consistent bulk density and phase purity, resolving the reliability issue while maintaining manufacturing feasibility

Inventive Principle:
Principle #36Phase transitions

2Manufacturing precision

If conventional manufacturing processes are used, then production can continue with existing methods, but bulk density varies leading to inconsistent dosing and drug performance

Engineering Contradiction:
Improvebulk density consistencyVSAvoidprocess control requirements
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

By changing the solvent parameter to DMSO and controlling the evaporation rate, the patent achieves consistent bulk density for Form III. This parameter modification standardizes the crystallization process, ensuring uniform particle packing and density without requiring complex real-time control systems, thus resolving the contradiction between precision and complexity

Inventive Principle:
Principle #35Parameter changes

3Productivity

If polymorphic forms are present in the product, then production can proceed without additional purification, but solubility variations occur resulting in side effects and reduced biological effectiveness

Engineering Contradiction:
Improveproduction efficiencyVSAvoidside effects
Core Design Contradiction:
ProductivityVSObject-generated harmful factors

Solution Approach 1:

The patent employs controlled phase transition through solvent evaporation to ensure exclusive formation of Form III crystals. This controlled transition prevents the formation of mixed polymorphic forms that would cause solubility variations and side effects, while maintaining high production efficiency by integrating the purification into the crystallization step itself

Inventive Principle:
Principle #36Phase transitions

Solution Approach 2:

By modifying the crystallization parameters (using DMSO solvent and controlled evaporation), the patent ensures selective formation of Form III with consistent solubility characteristics. This parameter control eliminates the harmful effect of polymorphic mixtures while maintaining productive manufacturing rates

Inventive Principle:
Principle #35Parameter changes

4Duration of action of stationary object

If extended storage is intended to maximize shelf life, then economic benefits are achieved, but phase transformation risk increases particularly when wetted with solvents

Engineering Contradiction:
Improveshelf lifeVSAvoidphase purity stability
Core Design Contradiction:
Duration of action of stationary objectVSStability of the object's composition

Solution Approach 1:

The patent creates a thermodynamically stable Form III that resists phase transformation during storage. The controlled crystallization from DMSO produces a stable polymorphic form that maintains its structure even when exposed to moisture or solvents during the intended shelf life, thus resolving the contradiction between extended storage duration and compositional stability

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

Form III exhibits enhanced bulk density and storage stability, maintaining phase purity even in the presence of solvents, leading to improved pharmaceutical processing and biological effectiveness with reduced side effects and extended shelf life.

Implementation Method 1

dissolution in DMSO

Methodology Applied
Scientific EffectSolvation: Solvation

Implementation Method 2

evaporation

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 3

X-ray powder diffraction patterns

Methodology Applied
Scientific EffectX-ray diffraction: X-Ray

Implementation Method 4

X-ray powder diffraction pattern expressed in D or 2-theta values

Methodology Applied
Scientific EffectBragg diffraction: Bragg Diffraction

Data Source

PatentEP3233807B1Crystalline form of 5-amino-2,3-dihydrophthalazine-1,4-dion sodium salt, pharmaceutical preparations containing the same and method for the production of said form
Publication Date: 2019.09.04 METRIOPHARM AG
  • EP3233807B1 patent drawingFigure 1a
  • EP3233807B1 patent drawingFigure 1b
  • EP3233807B1 patent drawingFigure 2a~2aIII

AI summary

The invention relates to the provision of a new crystalline form of 5-amino-2,3-dihydrophthalazine-1,4-dione sodium salt, a use of this form for medical purposes, methods for the production of the crystalline form according to the invention and to pharmaceutical preparations containing them.