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`UNITED STATES PATENT AND TRADEMARK OFFICE
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`BEFORE THE PATENT TRIAL AND APPEAL BOARD
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`FRESENIUS KABI USA, LLC and FRESENIUS KABI SWISSBIOSIM GmbH
`Petitioners,
`
`v.
`
`AMGEN, INC. and AMGEN MANUFACTURING LIMITED
`Patent Owners.
`
`
`IPR2020-00314
`
`Patent No. 9,856,287
`
`Title: REFOLDING PROTEINS USING A CHEMICALLY CONTROLLED
`REDOX STATE
`
`
`UPDATED EXHIBIT LIST
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`UPDATED LIST OF EXHIBITS
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`EXHIBIT NO.
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`DESCRIPTION
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`1001
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`1002
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`1003
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`1004
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`1005
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`1006
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`1007
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`1008
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`1009
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`1010
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`1011
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`1012
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`1013
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`1014
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`United States Patent No. 9,856,287
`
`Declaration of Professor Paul A. Dalby, Ph.D.
`
`United States Patent No. 4,237,224
`
`United States Patent No. 4,468,464
`
`United States Patent No. 4,740,470
`
`Curriculum Vitae of Professor Paul A. Dalby, Ph.D.
`De Bernardez Clark, E. et al., “Oxidative Renaturation of Hen
`Egg-White Lysozyme. Folding vs Aggregation,” Biotechnology
`Progress 14(1):47-54 (1998)
`De Bernardez Clark, E., “Protein refolding for industrial
`processes,” Current Opinion in Biotechnology 12(2):202-07
`(April 2001)
`Ejima, D. et al., “High Yield Refolding and Purification Process
`for Recombinant Human Interleukin-6 Expressed in Escherichia
`coli,” Biotechnology and Bioengineering, 62(3):301-10
`(February 1999)
`Excerpts of United States Patent No. 9,856,287 File History
`Ferrer-Miralles, N. et al., “Microbial factories for recombinant
`pharmaceuticals,” Microbial Cell Factories 8:17 (2009)
`Georgiou, G. & Valax, P., “Isolating Inclusion Bodies from
`Bacteria,” Methods in Enzymology 309:48-58 (1999)
`Gilbert, H., “Molecular and Cellular Aspects of Thiol-Disulfide
`Exchange,” in Advances in Enzymology and Related Areas of
`Molecular Biology, ed. Alton Meister, Vol. 63, pp. 69-172 (John
`Wiley & Sons 1990)
`Gilbert, H., “Thiol/Disulfide Exchange Equilibria and Disulfide
`Bond Stability,” in Methods in Enzymology, ed. Lester Packer,
`Vol. 251, pp. 8-28 (Academic Press 1995)
`
`1
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`
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`EXHIBIT NO.
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`1015
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`1016
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`1017
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`1018
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`1019
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`1020
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`1021
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`1022
`
`1023
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`1024
`
`1025
`
`1026
`
`1027
`
`
`
`DESCRIPTION
`Graumann, K. & Premstaller, A., “Manufacturing of
`recombinant therapeutic proteins in microbial systems,”
`Biotechnology Journal 1:164-86 (2006)
`Hevehan, D, & Clark, E., “Oxidative Renaturation of Lysozyme
`at High Concentrations,” Biotechnology and Bioengineering,
`54(3):221-30 (May 1997)
`Horton, R. et al., Principles of Biochemistry ( Pearson
`Education, 4th ed., 2006)
`Jungbauer, A. & Kaar, W., “Current status of technical protein
`refolding,” Journal of Biotechnology 128:587-96 (2007)
`Keire, D. et al., “Kinetics and Equilibria of Thiol/Disulfide
`Interchange Reactions of Selected Biological Thiols and Related
`Molecules with Oxidized Glutathione,” J. Org. Chem. 57(1):123-
`27 (1992)
`Neubauer, P. et al., “Protein Inclusion Bodies in Recombinant
`Bacteria,” in Inclusions in Prokaryotes, ed. J.M. Shively, pp.
`237-92 (Springer-Verlag Berlin Heidelberg 2006)
`Palmer, I. & Wingfield, P., “Preparation and Extraction of
`Insoluble (Inclusion-Body) Proteins from Escherichia coli, Curr
`Protoc Protein Sci. Chapter: Unit-6.3 (November 2004)
`Panda, A., “Bioprocessing of Therapeutic Proteins from the
`Inclusion Bodies of Escherichia coli,” Adv Biochem
`Engin/Biotechnol 85:43-93 (2003)
`Patra, A. et al., “Optimization of Inclusion Body Solubilization
`and Renaturation of Recombinant Human Growth Hormone
`from Escherichia coli,” Protein Expression and Purification
`18:182-92 (2000)
`Profacgen, “Inclusion body purification & protein refolding,”
`accessed at https://www.profacgen.com/inclusion-body-
`purification-protein-refolding.htm
`International Publication No. WO 95/32216
`Ryan, R. et al., “Structure-Function Relationships of
`Gonadotropins,” in Recent Progress in Hormone Research, Vol.
`43, pp. 383-429 (Academic Press 1987)
`Schafer, F. & Buettner, G., “Redox Environment of the Cell as
`Viewed Through the Redox State of the Glutathione
`
`2
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`EXHIBIT NO.
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`1028
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`1029
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`1030
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`1031
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`1032
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`1033
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`1034
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`1035
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`1036
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`1037
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`1038
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`1039
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`1040
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`1041
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`1042
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`
`
`DESCRIPTION
`Disulfide/Glutathione Couple,” Free Radical Biology &
`Medicine 30(11):1191-12 (June 2001)
`United States Patent Application Publication No. 2007/0238860
`Singh, S. & Panda, A., “Solubilization and Refolding of
`Bacterial Inclusion Body Proteins,” Journal of Bioscience and
`Bioengineering 99(4):303-10 (2005)
`Vallejo, L. & Rinas, U., “Strategies for the recovery of active
`proteins through refolding of bacterial inclusion body proteins,”
`Microbial Cell Factories 3:11 (2004)
`European Patent Application No. 1 449 848 A1, Method for the
`production of cystine-knot proteins (2004)
`Ventura, S. & Villaverde, A., “Protein quality in bacterial
`inclusion bodies,” Trends in Biotechnology 24(4):179-85 (April
`2006)
`Wetlaufer, D. et al., “The oxidative folding of proteins by
`disulfide plus thiol does not correlate with redox potential,”
`Protein Engineering 1(2):141-46 (1987)
`Whitford, D., Proteins: Structure and Function (John Wiley &
`Sons 2005)
`Peptides Guide, “What are Proteins?” accessed at
`http://www.peptidesguide.com/proteins.html
`Xie, Y. et al., “Recombinant Human Retinol-Binding Protein
`Refolding, Native Disulfide Formation, and Characterization,”
`Protein Expression and Purification 14:31-37 (1998)
`Patent Owner’s Preliminary Response Under 37 C.F.R. § 42.207,
`dated January 23, 2019
`Final Written Decision in IPR2016-01542, Patent 8,952,138,
`dated February 15, 2018
`Archer, D. et al., “Hen Egg White Lysozyme Expressed In, and
`Secreted from, Aspergillus Niger is Correctly Processed and
`Folded,” Bio/Technology 8:741-45 (August 1990)
`United States Patent No. 5,663,304
`
`United States Patent No. 8,952,138
`De Bernardez Clark, E., “Refolding of recombinant proteins,”
`Current Opinion in Biotechnology 9:157-63 (1998)
`
`3
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`EXHIBIT NO.
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`DESCRIPTION
`
`1043
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`1044
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`1045
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`1046
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`1047
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`1048
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`
`
`
`Atassi, M.Z., “Chemical Strategy for Studying the Antigenic
`Structures of Disulfide-Containing Proteins: Hen Egg-White
`Lysozyme as a Model,” in Protein Crosslinking, ed. M.
`Friedman, Vol. 6, pp. 89-137 (Plenum Press 1977)
`Table of categorized claims for United States Patent No.
`9,856,287
`“Glutathione” in The Merck Index, 12th Ed., pp. 4483-84 (Merck
`Research Laboratories 1996)
`Middleberg, A., “Preparative protein folding,” TRENDS in
`Biotechnology 20(10):437-43 (October 2002)
`Redline Petition IPR2019-00917/Petition IPR2020-000314
`
`Settlement Agreement [CONFIDENTIAL]
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`4
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`CERTIFICATE OF SERVICE
`
`The undersigned hereby certifies that copies of Petitioners’ UPDATED
`
`EXHIBIT LIST and EXHIBIT 1048 have been served in their entirety by causing
`
`the aforementioned documents to be electronically mailed to the following
`
`attorneys of record for the Patent Owner listed below:
`
`Patent Owner's Counsel of Record:
`
`Megan Raymond (Reg. No. 72,997)
`mraymond@paulweiss.com
`
`J. Steven Baughman (Reg. No. 47,414)
`sbaughman@paulweiss.com
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`Dated: June 18, 2020
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`Respectfully Submitted,
`
`By:
`
`
`/Huiya Wu/
`
`5
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`
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