Triazolopyrimidine Crystalline Forms Solubility and Residual Solvent Control

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

The existing pharmaceutical composition of N-((5-Fluoro-2,3-dihydrobenzofuran-4-yl)methyl)-8-(2-methylpyridin-3-yl)-[1,2,4]triazolo[4,3-c]pyrimidin-5-amine hydrochloride, known as Compound X, faces challenges with low aqueous solubility, variable crystallinity, and residual organic solvent contamination, particularly isopropanol, which affects its bioavailability and storage stability.

Innovation Solution

Development of crystalline forms, specifically Forms A, H A, and H B, using solvent combinations like EtOH/water and acetone/water, which enhance solubility, reduce residual solvent content, and improve crystallinity, allowing for consistent production and increased bioavailability.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If isopropanol is used as the manufacturing solvent for Compound X, then the compound can be produced, but residual isopropanol contamination occurs affecting bioavailability and storage stability

Engineering Contradiction:
Improvemanufacturing processVSAvoidresidual solvent contamination
Core Design Contradiction:
Ease of manufactureVSObject-affected harmful factors

Solution Approach 1:

The patent changes the solvent parameter from isopropanol to ethanol/water or acetone/water mixtures. This parameter change resolves the contradiction by eliminating residual isopropanol contamination while maintaining manufacturability. The new solvent system produces Compound X with reduced residual solvent levels, improving bioavailability and storage stability without compromising the manufacturing process.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent employs a disposable solvent system where ethanol/water or acetone/water are used and completely removed through evaporation and drying. These solvents serve their purpose during manufacturing and are then eliminated, leaving no harmful residues. This approach replaces the problematic isopropanol system with a cleaner, more suitable solvent that can be fully removed.

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

2Ease of manufacture

If conventional solid forms of Compound X are used, then production is simplified, but low aqueous solubility and variable crystallinity reduce bioavailability

Engineering Contradiction:
Improveproduction processVSAvoidbioavailability
Core Design Contradiction:
Ease of manufactureVSReliability

Solution Approach 1:

The patent changes the physical state parameter of Compound X from conventional solid forms to specifically defined crystalline forms (Forms A, HA, and HB). Each form has defined crystal structure characteristics that ensure consistent crystallinity and improved aqueous solubility. This parameter change resolves the contradiction by providing reliable bioavailability through controlled crystallinity while maintaining production simplicity.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent creates composite crystalline structures with specific molecular arrangements and intermolecular interactions. The crystalline forms represent organized composite structures of Compound X molecules in specific spatial configurations, which provide both consistent crystallinity and improved solubility properties while maintaining manufacturing ease.

Inventive Principle:
Principle #40Composite materials

3Reliability

If multiple solid forms (polymorphs) are considered for Compound X, then solubility and stability can be optimized, but selection complexity increases

Engineering Contradiction:
Improvesolubility and stabilityVSAvoidsolid form selection
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent segments the solid forms of Compound X into three distinct, well-defined crystalline forms (Forms A, HA, and HB), each with specific characterization parameters. This segmentation resolves the contradiction by providing clear, discrete options with defined properties, making selection straightforward based on specific solubility and stability requirements rather than dealing with undefined polymorphic variability.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The patent defines specific parameter ranges for each crystalline form (XRPD patterns, DSC transitions, solubility values) that serve as selection criteria. By establishing these parameter specifications, the patent simplifies the selection process - manufacturers can choose the appropriate form by matching their needs to the defined parameter profiles of Forms A, HA, or HB, reducing complexity while ensuring optimized performance.

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 crystalline forms of Compound X achieve improved bioavailability, dose-proportional exposure, and reduced residual solvent levels, addressing the issues of low solubility and variable crystallinity, thereby enhancing its therapeutic efficacy and storage stability.

Implementation Method 1

Development of crystalline forms, specifically Forms A, H A, and H B, using solvent combinations like EtOH/water and acetone/water, which enhance solubility, reduce residual solvent content, and improve crystallinity

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentEP3472168B1Crystalline forms of triazolopyrimidine compound
Publication Date: 2024.01.10 NOVARTIS AG
  • EP3472168B1 patent drawingFigure 1
  • EP3472168B1 patent drawingFigure 2
  • EP3472168B1 patent drawingFigure 3

AI summary

Provided herein are crystalline forms of a triazolopyrimidine compound, which is useful for treating a PRC2-mediated disease or disorder.