Balogh G, Tuba Z
Richter Gedeon Vegyészeti Gyár Rt., Budapest.
Acta Pharm Hung. 1992 May;62(3):97-102.
The synthesis of Pipecuronium bromide together with the investigation of its impurity profile required the solution of a number of analytical and structural problems. NMR spectroscopical methods received a major role in the structure elucidation of the synthesized compounds. The quantitative assessment of contaminations was also realized by 1H NMR spectroscopy. Out of the large amount of undertaken investigations, here we provide the structural characterization of the contaminating regiosimers of an important intermediate (5 alpha-androst-2-en-17-on) formed in the course of the synthesis, together with the NMR signal assignments of the end-product (Pipecuronium bromide) as measured in D2O and a mixture of CDCl3/DMSO-d6. The structure of a minor contamination of the end-product is also given.
合成哌库溴铵并研究其杂质概况需要解决一些分析和结构问题。核磁共振光谱法在合成化合物的结构解析中发挥了主要作用。通过¹H核磁共振光谱法也实现了对污染物的定量评估。在大量已开展的研究中,我们在此提供了合成过程中形成的一种重要中间体(5α-雄甾-2-烯-17-酮)的区域异构体污染物的结构表征,以及在D₂O和CDCl₃/DMSO-d₆混合物中测得的终产物(哌库溴铵)的核磁共振信号归属。还给出了终产物一种次要污染物的结构。