Synthesis of Formula I Compound via Adipic Acid Crystallization
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Solution Overview
Problem
The existing synthetic route for producing the compound of Formula (I) is inefficient for large-scale production due to its length, reliance on costly and unstable intermediates, and the need for expensive chromatography for purification.
Innovation Solution
A revised synthetic process that reduces the number of isolated intermediates, eliminates the use of costly compounds, and achieves sufficient purity for crystallization with adipic acid, allowing for large-scale production of the compound of Formula (I) without the need for chromatography.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Productivity
If the existing synthetic route (Scheme 1) is used, then the compound of Formula (I) can be produced on a laboratory scale, but the process is too long and complex for large-scale production
Solution Approach 1:
The synthesis route is divided into distinct modules: (a) preparation of compound of Formula (II) from commercially available starting materials, (b) conversion to compound of Formula (III), (c) conversion to compound of Formula (IV), and (d) final conversion to compound of Formula (I). This modular segmentation allows for optimized large-scale production while maintaining control over each transformation step.
Solution Approach 2:
The process performs preliminary actions by preparing and characterizing key intermediates (Formulas II, III, IV) in advance with defined purity specifications, allowing the final step to proceed efficiently without requiring extensive purification of earlier intermediates. The compound of Formula (II) is prepared with sufficient purity upfront to avoid later chromatography steps.
2Ease of manufacture
If the compound of Formula (A) is used as starting material, then the synthesis can proceed, but the cost is high and stability is poor
Solution Approach 1:
The invention replaces the expensive and unstable compound of Formula (A) with compound of Formula (II), which can be prepared from stable, commercially available starting materials. The new route uses readily available reagents and produces intermediates with sufficient stability for large-scale handling and storage, eliminating the need for costly and unstable Formula (A).
Solution Approach 2:
The process changes the chemical parameters by using different starting materials and reaction conditions. Instead of beginning with Formula (A) and its specific reaction requirements, the invention uses compound of Formula (II) prepared from stable starting materials with different reactivity profiles, allowing for more stable and cost-effective large-scale production.
3Manufacturing precision
If chromatography is used for purification, then the compound of Formula (I) can be purified, but the cost is expensive on large scale
Solution Approach 1:
The invention replaces the mechanical/chemical separation system of chromatography with a crystallization-based purification system. The compound of Formula (I) is purified through crystallization from appropriate solvents, which is a simpler, more scalable, and cost-effective method for large-scale production while achieving the required purity specifications.
Solution Approach 2:
The purification process utilizes phase transitions through crystallization. The compound of Formula (I) transitions from dissolved state in solvent to crystalline solid state, allowing for efficient separation and purification. This phase transition-based purification is inherently more scalable and cost-effective than chromatography for large-scale production.
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 improved process enables the production of the compound on a multikilogram scale, reducing costs and simplifying the purification process through crystallization with adipic acid, making it suitable for commercial production.
Implementation Method 1
The compound of Formula (I) is formed in sufficient purity that it can be isolated by crystallisation with adipic acid to form the adipic acid co-crystal of the compound of Formula (I)
Data Source
AI summary
A process and intermediates for making the compound of Formula (I). (I)