Automated Process Research and the Optimization of the Synthesis of 4(5)-(3-Pyridyl)imidazole
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Abstract
Automated process development technology was applied to the synthesis of 4(5)-(3-pyridyl)imidazole. This method utilizes automated liquid handling equipment coupled with statistically designed protocols for rapid process optimization. Two experimental sets were carried out based on a three-level factorial and central composite designs to optimise the product yield. The central composite design was repeated on one-fifth the scale to test the capabilities of the automated equipment. The reaction variables investigated were temperature and stoichiometry of formamide. The optimum in situ yield of 4(5)-(3-pyridyl)imidazole was found to be at 160 °C and 9 equiv of formamide. The results from the automated technology can be applied to larger-scale synthesis of the desired compound.
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