Project Goal:

Conduct a feasibility study on a synthesis of two process impurities for a customer who had contracted the project to another CRO prior to CalChem and obtained failed results.

Details:

The process involved an oxidation step, which resulted in the formation of a multi-component mixture due to a serious stability issue with the target molecules.
Neither a procedure to synthesize the compounds nor an HPLC method to monitor the reactions was provided by the customer.

Outcomes:

CalChem screened different reaction conditions and identified the most robust conditions to synthesize the compounds. HPLC method development was conducted alongside with the synthesis and a proper method was identified to monitor the reactions and assess the purities.   The ultimate conditions were utilized to prepare the requested amount of the two impurities within one month.  Overall, CalChem was able to develop a scalable and reproducible process for the synthesis of the two process impurities in high yield and excellent purity within a short period of time.