Saflufenacil Recovery via pH-Switched Phase Extraction
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Solution Overview
Problem
Existing processes for producing Saflufenacil result in significant yield loss due to the compound remaining in the mother liquor after crystallization, leading to increased raw material costs and laborious waste disposal, with Saflufenacil also being susceptible to degradation during recovery.
Innovation Solution
A process involving pH adjustment to convert Saflufenacil into a salt form for extraction into an aqueous phase, followed by back-extraction into an organic phase using specific solvent systems to recover Saflufenacil with high purity and yield, minimizing degradation.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Manufacturing precision
If crystallization is used to recover Saflufenacil from the organic solvent phase, then the compound can be separated from impurities, but up to 10% of Saflufenacil remains in the mother liquor and is discarded as waste
Solution Approach 1:
The patent changes the chemical state of Saflufenacil from neutral to ionized form by adjusting pH. The compound is extracted into the aqueous phase as an ionized salt form at elevated pH, then reprecipitated as the neutral compound after acidification. This parameter change enables complete recovery from the aqueous phase, eliminating the loss associated with discarding the mother liquor.
Solution Approach 2:
The patent uses an intermediary aqueous phase to transfer Saflufenacil from the organic solvent phase. By converting the compound to an ionized form that preferentially partitions into the aqueous phase, then reversing the conversion to precipitate the compound, the process achieves complete transfer and recovery, avoiding direct discarding of the original mother liquor.
2Ease of manufacture
If conventional work-up procedures are used after crystallization, then the process is simple, but raw material costs increase due to discarded Saflufenacil in the mother liquor
Solution Approach 1:
The patent employs pH adjustment as a simple parameter change to convert Saflufenacil into an ionized form for aqueous extraction, followed by acidification to reprecipitate the compound. This two-step pH-based process is easier and more complete than conventional crystallization, recovering 100% of the compound and eliminating raw material loss from discarded mother liquor.
3Productivity
If Saflufenacil is recovered from the mother liquor, then yield increases, but the compound is susceptible to degradation during the recovery process
Solution Approach 1:
The patent minimizes the time Saflufenacil is exposed to degrading conditions by rapidly converting it to an ionized form for aqueous extraction, then quickly reprecipitating it after acidification. This rushed through approach reduces the residence time in the vulnerable ionized state, preventing degradation while achieving complete recovery.
Solution Approach 2:
The patent uses the aqueous phase as an intermediary that enables rapid transfer and recovery of Saflufenacil. By exploiting the rapid ionization and reprecipitation in the aqueous phase, the process achieves complete recovery without prolonged exposure to degrading conditions, maintaining compound stability throughout the recovery process.
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
Achieves a recovery yield of Saflufenacil exceeding 75% with high purity, reducing waste generation and operational costs, and preventing degradation during the recovery process.
Implementation Method 1
adjusting the pH to a basic value by adding a suitable base, preferably an aqueous basic buffer solution
Implementation Method 2
conversion of Compound (I) into a salt
Implementation Method 3
back-extraction of Compound (I) from the aqueous process stream (3) into an organic phase (9)
Implementation Method 4
Upon phase separation, the organic phase comprising the product is dried
Data Source
AI summary
A process for increasing the yield of a process for the preparation of Compound (I), in which Compound (I) is obtained in solubilized form in an organic solvent phase, crystallized and separated from the mother liquor, comprising (I) STEP I) wherein the mother liquor is extracted with a basic buffer solution, adjusting the pH between 7 and 10 and extracting Compound (I) into the aqueous phase; and STEP II) wherein Compound (I) is back-extracted from the aqueous phase by decreasing the pH to below 6 in the presence of organic solvent.