Anhydrous BTK Inhibitor Polymorphs for Stable Solid-State Selection

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Solution Overview

Problem

There is a need to provide a solid state form of N-(3-(6-Amino-5-(2-(N-methylacrylamido)ethoxy)pyrimidin-4-yl)-5-fluoro-2-methylphenyl)-4-cyclopropyl-2-fluorobenzamide that possesses physicochemical properties allowing for a reliable production of a safe and efficacious drug product, as existing knowledge does not account for crystalline forms of this BTK inhibitor.

Innovation Solution

The development of crystalline forms A, B, and C of N-(3-(6-Amino-5-(2-(N-methylacrylamido)ethoxy)pyrimidin-4-yl)-5-fluoro-2-methylphenyl)-4-cyclopropyl-2-fluorobenzamide, which are characterized by specific XRPD patterns, thermal profiles, and methods of preparation such as anti-solvent crystallization, cooling crystallization, or solvent evaporation.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If multiple crystalline forms are discovered, then stability and solubility can be optimized, but the complexity of selecting and characterizing the appropriate form increases

Engineering Contradiction:
ImprovestabilityVSAvoidcomplexity of selecting and characterizing crystalline form
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent segments the complex problem of solid-state characterization by dividing it into distinct crystalline forms (Form A, Form B, Form C), each with specific XRPD patterns and properties. This segmentation allows systematic evaluation of each form's stability and solubility characteristics independently, making the overall selection process more manageable.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The patent applies parameter changes by varying crystallization conditions (solvent type, temperature, evaporation rate) to generate different crystalline forms. By systematically changing these parameters, the inventors were able to discover and characterize multiple polymorphs with different properties, enabling optimization of stability and solubility.

Inventive Principle:
Principle #35Parameter changes

2Measurement precision

If crystalline forms are characterized using multiple analytical methods, then accurate identification and property determination are achieved, but the time and resources required increase

Engineering Contradiction:
Improveaccuracy of crystalline form identificationVSAvoidtime required for characterization
Core Design Contradiction:
Measurement precisionVSLoss of time

Solution Approach 1:

The patent employs preliminary action by establishing a hierarchical characterization approach where XRPD patterns are used as the primary identification tool due to their rapid and definitive nature. Once a crystalline form is identified via XRPD, subsequent characterization (DSC, TGA, solubility studies) is focused on that specific form, reducing overall time compared to comprehensive analysis of all possible forms.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent applies universality by using a core set of analytical methods (XRPD, DSC, TGA) that serve multiple purposes: XRPD identifies crystalline form and monitors phase purity, DSC provides thermal stability data and polymorph identification, and TGA assesses solvate/hydrate content. This multi-functional approach reduces the need for additional specialized tests.

Inventive Principle:
Principle #6Universality (Multi-functionality)

3Reliability

If the preferred crystalline form is selected based on optimal properties, then drug efficacy and safety are improved, but the difficulty of predicting which form will be optimal increases

Engineering Contradiction:
Improvedrug efficacyVSAvoiddifficulty of predicting optimal crystalline form
Core Design Contradiction:
ReliabilityVSDifficulty of detecting and measuring

Solution Approach 1:

The patent applies preliminary action by conducting comprehensive screening of multiple crystalline forms early in the development process. By preparing and characterizing Forms A, B, and C beforehand, the team established a database of properties (solubility, stability, melting point) that enables informed selection of the optimal form for drug development, avoiding later surprises.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent uses computational chemistry and molecular modeling as intermediaries to predict which crystalline forms are likely to form and what their properties might be. These computational tools serve as intermediaries between the molecular structure of the BTK inhibitor and the observed properties of its polymorphs, providing guidance on which forms to prioritize for synthesis and testing.

Inventive Principle:
Principle #24Intermediary (Mediator)

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 crystalline forms exhibit improved stability, solubility, and bioavailability, enabling effective treatment of BTK-mediated disorders, including autoimmune and inflammatory diseases, with potential for phase purity and therapeutic efficacy.

Implementation Method 1

methods of preparation such as anti-solvent crystallization, cooling crystallization, or solvent evaporation

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentEP3972960B1Crystalline forms of a BTK inhibitor
Publication Date: 2025.12.24 NOVARTIS AG
  • EP3972960B1 patent drawingFigure 1
  • EP3972960B1 patent drawingFigure 2
  • EP3972960B1 patent drawingFigure 3

AI summary

This application relates to various anhydrous crystalline forms N-(3-(6-Amino-5-(2-(N-methylacrylamido)ethoxy)pyrimidin-4-yl)-5-fluoro-2-methylphenyl)-4-cyclopropyl-2-fluorobenzamide, as well as compositions, method of making and methods of using the same.These crystalline forms are useful in the treatment of diseases and disorders which are typically ameliorated by the inhibition of BTK. Such diseases and disorders may include inflammatory and autoimmune disorders and pulmonary and respiratory tract inflammation.