Crystalline Form I Monohydrate Stability via Hydration

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Solution Overview

Problem

There is a need for more stable forms of 4-[(2,4-dichloro-5-methoxyphenyl)amino]-6-methoxy-7-[3-(4-methyl-1-piperazinyl)propoxy]-3-quinolinecarbonitrile that maintain high solubility, as existing forms are prone to degradation and have variable stability.

Innovation Solution

The development of crystalline Form I, a monohydrate with a specific x-ray diffraction pattern, which is more stable and has a higher transition temperature, achieved through treatment of anhydrous Form V with heated water or at room temperature, converting other polymorphs into Form I using water.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If existing crystalline forms are used, then the compound can be supplied for pharmaceutical use, but the forms are prone to degradation and have variable stability

Engineering Contradiction:
ImprovestabilityVSAvoiddegradation resistance
Core Design Contradiction:
ReliabilityVSStability of the object's composition

Solution Approach 1:

The patent applies parameter changes by identifying and characterizing different polymorphic forms (Form I through Form VI) of the compound, each with distinct crystal structures, stability profiles, and physical properties. Form I is specifically identified as the most stable polymorph with defined XRD patterns and transition temperatures, resolving the stability issue by selecting and controlling for this specific crystalline parameter configuration

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs composite material principles by creating a monohydrate form (Form I) that incorporates water molecules into the crystal lattice structure. This composite approach, where the compound forms a stable hydrate complex, enhances the overall stability and reliability of the pharmaceutical material compared to anhydrous forms

Inventive Principle:
Principle #40Composite materials

2Stability of the object's composition

If more stable crystalline forms are developed, then degradation resistance improves, but maintaining high solubility becomes challenging

Engineering Contradiction:
Improvedegradation resistanceVSAvoidsolubility
Core Design Contradiction:
Stability of the object's compositionVSQuantity of substance

Solution Approach 1:

The patent resolves this contradiction by systematically evaluating multiple polymorphic forms with different physical parameters. Form I is identified as having the optimal balance, exhibiting both high stability (transition temperature 109-115°C) and maintained solubility characteristics, demonstrating that parameter optimization can achieve both stability and solubility requirements simultaneously

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

Form I exhibits enhanced stability, retaining purity and physical integrity under various environmental conditions, including high humidity, temperature, and light exposure, with a transition temperature range of 109°C to 115°C, making it more desirable for pharmaceutical applications.

Implementation Method 1

One method of preparing 4-[(2,4-dichloro-5-methoxyphenyl)amino]-6-methoxy-7-[3-(4-methyl-1-piperazinyl)propoxy]-3-quinolinecarbonitrile monohydrate (Form I) comprises the step of treating anhydrous 4-[(2,4-dichloro-5-methoxyphenyl)amino]-6-methoxy-7-[3-(4-methyl-1-piperazinyl)propoxy]-3-quinolinecarbonitrile, known herein as Form V, with heated water

Methodology Applied
Scientific EffectHydration: Hydrates

Implementation Method 2

One method of preparing 4-[(2,4-dichloro-5-methoxyphenyl)amino]-6-methoxy-7-[3-(4-methyl-1-piperazinyl)propoxy]-3-quinolinecarbonitrile monohydrate (Form I) comprises the step of treating anhydrous 4-[(2,4-dichloro-5-methoxyphenyl)amino]-6-methoxy-7-[3-(4-methyl-1-piperazinyl)propoxy]-3-quinolinecarbonitrile, known herein as Form V, with heated water

Methodology Applied
Scientific EffectHeating: Heating

Implementation Method 3

The polymorph is a monohydrate (Form I) having an x-ray diffraction pattern wherein all of the 2θ angles (°) of significant peaks are either at about: 9.19, 11.48, 14.32, 19.16, 19.45, 20.46, 21.29, 22.33, 23.96, 24.95, 25.29, 25.84, 26.55, 27.61, and 29.51

Methodology Applied
Scientific EffectX-ray diffraction: X-Ray

Data Source

PatentEP1902029B2Crystalline forms of 4-[(2,4-dichloro-5-methoxyphenyl)amino]-6-methoxy-7-[3-(4-methyl-1-piperazinyl)propoxy]-3-quinolinecarb-onitrile and methods of preparing the same
Publication Date: 2022.02.16 WYETH LLC
  • EP1902029B2 patent drawingFigure 1
  • EP1902029B2 patent drawingFigure 2
  • EP1902029B2 patent drawingFigure 3

AI summary

This invention is directed to a crystalline 4-[(2,4-dichloro-5- methoxyphenyl)amino]-6-methoxy-7-[3-(4-methyl-l-piperazinyl)propoxy]-3- quinolinecarbonitrile monohydrate having an x-ray diffraction pattern wherein 20 angles (°) of significant peaks are at about: 9.19, 11.48, 14.32, 19.16, 19.45, 20.46, 21.29, 22.33, 23.96, 24.95, 25.29, 25.84, 26.55, 27.61, and 29.51, and a transition temperature of about 109ºC to about 115ºC.