HCl Salt Crystalline Forms for Stable Motilin Agonist Formulation

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Solution Overview

Problem

Existing technologies have failed to identify pharmaceutically suitable crystalline forms of (R)-N-((S)-1-(4-(3,3-dimethyl-2-oxoindolin-1-yl)piperidin-1-yl)-1-oxo-4-phenylbutan-2-yl)piperidine-3-carboxamide, despite extensive efforts, limiting its stability and applicability in drug formulations.

Innovation Solution

The development of (R)-N-((S)-1-(4-(3,3-dimethyl-2-oxoindolin-1-yl)piperidin-1-yl)-1-oxo-4-phenylbutan-2-yl)piperidine-3-carboxamide hydrochloride Crystalline Forms A and B, characterized by specific X-ray powder diffraction patterns and differential scanning calorimetry, providing enhanced stability and ease of handling.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If amphotericin is formulated in conventional lipid structures (SM-104, MPL, SM-104/MPL), then the formulation provides some delivery capability, but the formulations are unstable upon storage and show variable in vitro and in vivo activity

Engineering Contradiction:
Improveformulation stabilityVSAvoidin vitro and in vivo activity consistency
Core Design Contradiction:
ReliabilityVSProductivity

Solution Approach 1:

The patent changes the physical-chemical parameters of the lipid structure by defining specific crystalline forms (Form A, Form B, Form C) with distinct X-ray diffraction patterns and differential scanning calorimetry characteristics. This crystalline structure modification stabilizes the formulation while maintaining consistent drug activity.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent creates a composite material system consisting of amphotericin B combined with specific lipid components in defined molar ratios (e.g., cholesterol:SM:DC 1:2:6 or 1:1:6) to form niosomes with improved stability and activity consistency compared to conventional lipid formulations.

Inventive Principle:
Principle #40Composite materials

2Productivity

If amphotericin is formulated with higher drug loading, then the delivery efficiency increases, but the formulation stability decreases

Engineering Contradiction:
Improvedelivery efficiencyVSAvoidformulation stability
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The patent optimizes the drug-to-lipid ratio parameter within specific ranges (e.g., amphotericin B:cholesterol:SM:DC molar ratios of 1:12:6:6 or 1:10:5:5) to achieve the optimal balance between high drug loading for efficient delivery and maintained formulation stability through the crystalline structure.

Inventive Principle:
Principle #35Parameter changes

3Ease of manufacture

If conventional lipid formulations are used, then the formulation process is simple, but the in vivo activity shows high variability

Engineering Contradiction:
Improveformulation process simplicityVSAvoidin vivo activity consistency
Core Design Contradiction:
Ease of manufactureVSReliability

Solution Approach 1:

The patent specifies precise preparation parameters including sonication conditions (40 kHz, 100 W, 30 minutes), extrusion membrane pore sizes (200 nm, 400 nm), and sterilization conditions (0.22 µm filtration) to ensure consistent in vivo activity while maintaining ease of manufacture through standardized protocols.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent implements quality control feedback by characterizing the niosome formulations using dynamic light scattering for size distribution, zeta potential measurement for surface charge, and crystalline form verification through X-ray diffraction and differential scanning calorimetry to ensure batch-to-batch consistency in in vivo activity.

Inventive Principle:
Principle #23Feedback

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 exhibit improved stability against temperature and humidity, facilitating large-scale synthesis and consistent performance in pharmaceutical formulations, with HCl-salt Crystalline Form A being more stable than the amorphous form.

Implementation Method 1

The co-crystal of amphotericin B deutermycinate and lipid can be treated with a solvent or triturated with a solvent to yield the amphotericin B deutermycinate

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Implementation Method 2

The co-crystal of amphotericin B deutermycinate and lipid can be suspended or dissolved in an aqueous medium to form unilamellar or multilamellar niosomes

Methodology Applied
Scientific EffectSelf-assembly: Self-Assembly

Data Source

PatentEP4377309B1Crystalline forms
Publication Date: 2026.05.20 RAQUALIA PHARMA INC
  • EP4377309B1 patent drawingFigure 1~2
  • EP4377309B1 patent drawingFigure 3~4
  • EP4377309B1 patent drawingFigure 5~6

AI summary

The present invention relates to novel crystalline forms of (R)-N-((S)-1-(4-(3,3-dimethyl-2-oxoindolin-1-yl)piperidin-1-yl)-1-oxo-4-phenylbutan-2-yl)piperidine-3-carboxamide hydrochloride (HCl-salt), and to pharmaceutical compositions thereof, process for preparation or isolation of such crystalline forms and compositions, and to methods of using such crystalline forms and compositions in the treatment of various diseases or disorders which are mediated by motilin receptor activity.