Identification of critical process impurities and their impact on process research and development

Organic Process Research and Development

Volumn 12, Issue 4, 2008, Pages 632-636

  Huang, Yande ^a   Ye, Qingmei ^a   Guo, Zhenrong ^a   Palaniswamy, Venkatapuram A ^a   Grosso, John A ^a  

^a BRISTOL MYERS SQUIBB   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 58149164692     PISSN: 10836160     EISSN: 1520586X     Source Type: Journal    
DOI: 10.1021/op800067v     Document Type: Article

References (11)

1. International Conference on Harmonisation (ICH) Guidelines; Q8, Pharmaceutical Development, 2005; Q9, Quality Risk Management, 2006.
2. Ganzer, W. R.; Materna, J. A.; Mitchell, M. B.; Wall, L. K. Pharm. Technol. 2005, (July 2), 1-12.
3. Nasr, M. Drug Information Association Annual Meeting, Philadelphia, PA, June 19, 2006; Pharmaceutical Quality Assessment System. (PQAS) in the 21st Century, 2006.
4. Stein, P. D.; Bisacchi, G. S.; Shi, Y.; O'Connor, S. P.; Li, C. PCT Int. Appl. WO 2000047207, 2000; Application: A1. 20000817; WO 2000-US2883, 2002.
5. Guo, Z.; Li, W.-S.; Dowdy, E.; Polniaszek, R.; Kant, J.; Miller, M. 224th ACS National Meeting, Boston, MA, United States, August 18-22, 2002; Improved preparation of 5-{N-(2-methyl-benzofuran-5-yl)-N -[2-oxo-1-(2-oxo- 2-pyrrolidin-1-yl-ethyl)-azepan-3-yl]-guanidinocarbonyl)-pyridine-2-carboxylic acid dim.ethylamide: A potent and selective Factor Xa Inhibitor Abstracts of Papers, 2002; ORGN-735.
6. International Conference on Harmonisation (ICH) Guidelines; Q3A(R), Impurities in New Drug Substances (Revised Guidelines), 2003.
7. 13C NMR chemical shifts assignments of impurity A are shown in Tables 1 and 2 in the Supporting Information.
8. 13C NMR chemical shifts assignments of impurity B are shown in Tables 3 and 4 in the Supporting Information.
9. 13C NMR chemical shifts assignments of impurity C are shown in Tables 5 and 6 in the Supporting Information.
10. LC/MS chromatograms of impurities C, E, and G and mass spectra of E and G are shown in Figures s2 and s3 in the Supporting Information.
11. LC/MS chromatogram and mass spectra of impurities D and F are shown in Figure s4 in the Supporting Information.