Crystalline AHU-377 Salt Solves Viscous Handling Bottleneck

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

The existing forms of AHU-377, a key component in LCZ696, are challenging to handle due to its viscous nature, leading to operational difficulties in industrial production, and there is a need for a stable solid form to enhance its quality, stability, and storage.

Innovation Solution

A crystalline form of AHU-377 is developed through a multi-step synthesis process involving reactions with specific reagents and solvents, resulting in a stable compound with defined X-ray powder diffraction patterns and improved handling properties.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of operation

If AHU-377 is used in its existing form, then the drug can exert its pharmacological effect, but the viscous nature causes operational difficulties in transfer and quantification during industrial production

Engineering Contradiction:
Improvehandling of AHU-377VSAvoidindustrial production efficiency
Core Design Contradiction:
Ease of operationVSProductivity

Solution Approach 1:

The patent changes the physical state parameter of AHU-377 from viscous liquid to crystalline solid through salt formation. This transformation fundamentally alters the material's handling properties, enabling easy transfer, quantification, and processing in industrial production while maintaining its pharmacological activity.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent creates a composite crystalline material by forming a salt between AHU-377 (a carboxylic acid) and a base. This composite crystalline form combines the pharmacologically active AHU-377 with a counterion, producing a stable solid that is easy to handle and process while retaining the original drug's therapeutic effects.

Inventive Principle:
Principle #40Composite materials

2Reliability

If AHU-377 is used in its existing viscous form, then the drug maintains its pharmacological activity, but the quality control and stability are compromised

Engineering Contradiction:
Improvestability of AHU-377VSAvoidhandling of viscous mass
Core Design Contradiction:
ReliabilityVSEase of operation

Solution Approach 1:

The patent transforms AHU-377 from a viscous liquid to a crystalline solid through salt formation, fundamentally changing its physical parameters. This transformation improves stability by establishing a defined crystal structure with consistent properties, while the crystalline form enables reliable quality control through standardized handling and measurement procedures.

Inventive Principle:
Principle #35Parameter changes

3Stability of the object's composition

If AHU-377 is stored in its viscous form, then the drug remains active, but storage conditions and handling become problematic

Engineering Contradiction:
Improvestability of AHU-377VSAvoidstorage and weighing
Core Design Contradiction:
Stability of the object's compositionVSEase of manufacture

Solution Approach 1:

The patent changes the physical state from viscous liquid to crystalline solid, which fundamentally improves storage characteristics. The crystalline form provides stability through its ordered structure and enables easy manufacturing operations including weighing, dosing, and storage under standard conditions without special precautions required for viscous materials.

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 form of AHU-377 exhibits improved stability, ease of handling, and high purity, facilitating industrial production and pharmaceutical applications, while also providing a stable basis for drug formulations.

Implementation Method 1

5-(biphenyl-4-yl)-4-[(tert-butoxycarbonyl)amino]-2-methylpentanoic acid is reacted with ethanol and thionyl chloride to give ethyl 5-([1,1-biphenyl)-4-amino-2- methylpentanoate hydrochloride

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

ethyl 5-([1,1-biphenyl)-4-amino-2-methylpentanoate hydrochloride is reacted with succinic anhydride in the presence of a base to give ethyl 5-(biphenyl-4-yl)-4-[(3-carboxypropionyl)amino]-2-methylpentanoate

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 3

ethyl 5-(biphenyl-4-yl)-4-[(3-carboxypropionyl)amino]-2-methylpentanoate is reacted with ammonia water (for example, concentrated ammonia water) or ammonia gas to give the compound of formula (A)

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 4

the X-ray powder diffraction pattern thereof has characteristic peaks at 2θ values of 10.04 ° ± 0.20 °, 16.66 ° ± 0.20 °, 21.89 ° ± 0.20 °

Methodology Applied
Scientific EffectX-ray diffraction: X-Ray

Data Source

PatentEP3611160B1Ammonium carboxylate compound, crystal form and amorphous substance thereof, and preparation method therefor
Publication Date: 2023.03.29 WUHAN LL SCI & TECH DEV CO LTD
  • EP3611160B1 patent drawingFigure 1~2
  • EP3611160B1 patent drawingFigure 3
  • EP3611160B1 patent drawingFigure 4~6

AI summary

The present disclosure belongs to the field of chemical synthesis, and in particular relates to an ammonium carboxylate compound, a crystalline form and an amorphous form, and a preparation method thereof. The present disclosure prepares the compound and the crystalline form I and its single crystal, amorphous form and crystalline form II thereof. The compound, the crystalline forms, the single crystal and the amorphous form can stably exist and exhibit good solid forms, suitable for medicine-making. Furthermore, these products possess high purity and less single impurity. Moreover, the preparation methods of the present disclosure are easy to implement due to the simple processes with mild reaction conditions, and could produce products of high yield and high purity without complex purification steps. Furthermore, the preparation methods may facilitate safety, environmental protection, and industrial production.