Automated Process Research and the Optimization of the Synthesis of 4(5)-(3-Pyridyl)imidazole

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• 作者：Eric W. Kirchhoff ; Denise R. Anderson ; Songlei Zhang ; Constance S. Cassidy ; and Michael T. Flavin
• 刊名：Organic Process Research & Development
• 出版年：2001
• 出版时间：January 2001
• 年：2001
• 卷：5
• 期：1
• 页码：50 - 53
• 全文大小：69K
• 年卷期：v.5,no.1(January 2001)
• ISSN：1520-586X

文摘

Automated process development technology was applied to thesynthesis of 4(5)-(3-pyridyl)imidazole. This method utilizesautomated liquid handling equipment coupled with statisticallydesigned protocols for rapid process optimization. Two experimental sets were carried out based on a three-level factorialand central composite designs to optimise the product yield.The central composite design was repeated on one-fifth the scaleto test the capabilities of the automated equipment. The reactionvariables investigated were temperature and stoichiometry offormamide. 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 tolarger-scale synthesis of the desired compound.