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`Merck Exhibit 2129, Page 1
`Mylan v. Merck, IPR2020-00040
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`Merck Exhibit 2129, Page 1
`Mylan v. Merck, IPR2020-00040
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`Merck Exhibit 2129, Page 1
`Mylan v. Merck, IPR2020-00040
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`Merck Exhibit 2129, Page 1
`Mylan v. Merck, IPR2020-00040
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`Merck Exhibit 2129, Page 2
`Mylan v. Merck, IPR2020-00040
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`Merck Exhibit 2129, Page 2
`Mylan v. Merck, IPR2020-00040
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`Merck Exhibit 2129, Page 3
`Mylan v. Merck, IPR2020-00040
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`Merck Exhibit 2129, Page 3
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`Merck Exhibit 2129, Page 4
`Mylan v. Merck, IPR2020-00040
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`Merck Exhibit 2129, Page 4
`Mylan v. Merck, IPR2020-00040
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`Merck Exhibit 2129, Page 5
`Mylan v. Merck, IPR2020-00040
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`Merck Exhibit 2129, Page 5
`Mylan v. Merck, IPR2020-00040
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`Merck Exhibit 2129, Page 6
`Mylan v. Merck, IPR2020-00040
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`Merck Exhibit 2129, Page 6
`Mylan v. Merck, IPR2020-00040
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`Mylan.v. Merck, IPR2020-00040
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`Merck Exhibit 2129, Page 7
`Mylan v. Merck, IPR2020-00040
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`Mylan v. Merck, IPR2020-00040
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`Merck Exhibit 2129, Page 10
`Mylan v. Merck, IPR2020-00040
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`
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`MERCK & CO.,.INC.,
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`pe[sebbaron
`
`Merck Exhibit 2129, Page 11
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 11
`Mylan v. Merck, IPR2020-00040
`
`
`
`Hansen, Karl
`
`i
`
`Wap
`
`rom:
`ent:
`To:
`
`Karl,
`
`Dorwart, Jason G.
`Tuesday, February 05, 2002 11:13 AM
`Hansen, Karl
`
`Here are the results of the L-224715 Besylate salt NB# 70316-001.
`
`LCAP
`RRT
`0.65
`0.93
`0.95
`1.00
`1.04
`1.37
`
`Area %
`0.06%
`0.16%
`0.20%
`99.27%
`0.09%
`0.13%
`
`Chiral
`Major Enantiomer = 99.92%
`Minor Enantiomer = 0.08%
`
`ir
`
`ason
`
`Merck Exhibit 2129, Page 12
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 12
`Mylan v. Merck, IPR2020-00040
`
`
`
`Data file
`
`:C:\HPCHEM\HPLCO157\DATA\005-0101.D
`
`Sample Name: 70316-001
`
`0.1900g/50m1 of hydrog soln 17.85 g
`
`->
`
`Injection Date : 01/30/2002
`Sample Name
`: 70316-0001
`Acq Operator
`: hansen
`
`12:29:35 PM
`
`Seq Line
`Vial No
`Inj. No.
`Inj. Vol.
`: C:\HPCHEM\HPLCO157\METHODS\715.M
`Method
`: 01/14/2002
`1:00:57 PM
`Last Changed
`75/25 0.1% HC104/Acetonitrile, 1ml/min
`
`10min 25/75 water/acn; 75/25 from 10 to 14 min
`
`:
`:
`:
`
`l
`5
`1
`2 pl
`
`ML QAx, otHH a
`
`waters cl8 symmetry, 250 nm
`
`DAD1 C, Sig=210,8 Ref=360,100 (005-0101.D)
`
`Sorted By
`Calib. Data Modified
`Multiplier
`
`>: Signal
`: 01/14/2002
`> 1.000000
`
`1:00:30 PM
`
`Signal:
`
`1 DAD1 C, Sig=210,8 Ref=360,100
`
`Peak
`+
`
`RT
`{min}
`
`Type Width Height
`(min)
`
`Area
`[mAU*s]
`
`Area
`%
`
`Amount
`mg/ml
`
`Name
`
`.88 BB
`
`0
`0.082
`0.078
`
`0.083
`0.091
`0.201
`
`65.94
`30.31
`
`1.06
`2.62
`24.14
`
`.
`350.924
`149.939
`
`5.689
`15.583
`308.655
`
`.
`41.82
`17.87
`
`0.68
`1.86
`36.78
`
`0.00000C
`0.08999C
`0.00000C
`
`0.Q00000C
`0.00000C
`0.00000C
`
`L-224,715
`Benzy alert
`
`Signal:
`
`2 DAD1 E, Sig=268,16 Ref=360,100
`
`Peak
`#
`
`RT
`[min}
`
`Type Width Height
`(min)
`
`Area
`[mAU*s]
`
`Area
`%
`
`Amount
`mg/ml
`
`Name
`
`5.55 BB
`1
`2 12.88 PB
`
`0.082
`0.204
`
`7.55
`1.86
`
`40.148
`24.616
`
`61.99
`38.01
`
`0.08999C
`0.00000C
`
`L-224,715
`
`HPLCO157
`
`01/30/2002
`
`12:43:56 PM
`
`Page 1 of 2
`Merck Exhibit 2129, Page 13
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 13
`Mylan v. Merck, IPR2020-00040
`
`
`
`Data file
`
`:C:\HPCHEM\HPLCO157\DATA\098-0101.D
`
`Sample Name: 70316-001
`
`methanol soln of hydrog after
`
`Injection Date : 01/29/2002
`Sample Name
`: 70316-0001
`Acq Operator
`: hansen
`
`8:26:05 AM
`
`Seq Line
`Vial No
`Inj. No.
`Inj. Vol.
`>: C:\HPCHEM\HPLCO157\METHODS\715.M
`Method
`: 01/14/2002
`1:00:57 PM
`Last Changed
`lml/min
`75/25 0.1% HC104/Acetonitrile,
`75/25 from 10 to 14 min
`10min 25/75 water/acn;
`waters cl8 symmetry, 250 nm
`
`©w
`
`oaw
`
`o
`
`DAD1 C, Sig=210,8 Ref=360,100 (098-0101.D)
`
`
`ooooooocoocooorqcoceomg/ml
`
`Sorted By
`Calib. Data Modified
`Multiplier
`
`Signal
`01/14/2002
`1.000000
`
`1:00:30 PM
`
`Signal:
`
`1 DAD] C, Sig=210,8 Ref=360,100
`
`Peak
`#
`
`RT
`(min)
`
`Type Width Height
`(min]
`
`Area
`
`[mAU*s]
`
`Amount
`
`2.28 BV
`1
`2.39 VB
`2
`2.96 BB
`3
`3.63 PB
`4
`5.55 BV
`5
`5.88 VV
`6
`6.13 VB
`7
`6.77 BB
`8
`7.46 PV
`9
`8.21 BV
`10
`8.35 VV
`11
`8.51 VP
`12
`9.90 BV
`13
`14 10.11 VB
`15 10.44 BB
`
`0.064
`0.074
`0.071
`0.080
`0.085
`0.078
`0.103
`0.080
`0.098
`0.099
`0.084
`0.085
`0.086
`0.116
`0.085
`
`ww NM oO
`
`rh
`
`000000
`.000000
`. 000000
`000000
`.276818
`.000000
`000000
`000000
`000000
`.000000
`-000000
`000000
`000000
`000000
`000000
`
`L-224,715
`
`HPLCO157
`
`01/29/2002
`
`Page 1 of 2
`Merck Exhibit 2129, Page 14
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 14
`Mylan v. Merck, IPR2020-00040
`
`
`
`Data file
`Peak
`#
`
`:C: \HPCHEM\HPLC0157\DATA\098-0101.D
`Area
`Area
`RT
`Type Width
`Height
`(min)
`(min]
`
`[mAU*s]
`
`%
`
`16 11.60 BB
`17 11.95 BV
`18 12.14 VB
`19 12.69 BV
`20 12.95 VV
`21 13.27 VV
`22 13.55 VB
`
`0.194
`0.105
`0.087
`0.123
`0.129
`0.185
`0.108
`
`3.70
`1.83e3
`8.67
`125.53
`58.48
`10.69
`
`33.466
`27.092
`9921.391
`76.832
`1132.982
`715.638
`79.096
`
`0.17
`0.13
`49.40
`0.38
`5.64
`3.56
`0.39
`
`. 000000
`000000
`. 000000
`000000
`000000
`000000
`.000000
`
`Signal:
`
`2 DAD1 E, Sig=
`
`268,16
`
`Ref=360,100
`
`Peak
`#
`
`RT
`{min]
`
`Type Width
`[min]
`
`Height
`
`Area
`(mAU*s]
`
`Area
`%
`
`566.822
`
`34.94
`
`5.55 BB
`1
`5.88 BB
`2
`6.77 BB
`3.
`4 12.14 BB
`5 12.97 VV
`6 13.27 VV
`7:13.55 VB
`
`0.082
`0.081
`0.082
`0.079
`0.175
`0.182
`0.104
`
`106.70
`5.96
`1.27
`173.36
`5.89
`5.19
`
`- 276818
`000000
`000000
`. 000000
`000000
`. 000000
`000000
`
`*** End of Report ***
`
`Sample Name: 70316-001
`Name
`
`L-224,715
`
`HPLCO157
`
`01/29/2002
`
`8:40:32 AM
`
`Page 2 of 2
`Merck Exhibit 2129, Page 15
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 15
`Mylan v. Merck, IPR2020-00040
`
`
`
`Data file
`
`:C:\HPCHEM\HPLC0157\DATA\099-0201.D
`
`Sample Name: 70316-001
`
`benzyl alcohol
`
`->
`
`8:44:40 AM
`
`Injection Date : 01/29/2002
`Sample Name
`: 70316-0001
`Acq Operator
`: hansen
`
`Seq Line
`Vial No
`Inj. No.
`Inj. Vol.
`: C:\HPCHEM\HPLCO157\METHODS\715.M
`Method
`: 01/14/2002
`1:00:57 PM
`Last Changed
`75/25 0.1% HC104/Acetonitrile,
`Iml/min
`10min 25/75 water/acn; 75/25 from 10 to 14 min
`waters cl8 symmetry, 250 nm
`
`2
`:
`: 99
`:
`1
`:
`2 pl
`
`DAD1 C, Sig=210,8 Ref=360,100 (099-0201.D)
`
`mAU
`
`xa
`
`
`
`4
`2
`0
`DAD1 E, Sig=268,16 Ref=360,100 (099-0201 D)
`
`6
`
`8
`
`10
`
`12
`
`14
`
`min
`
`mAU
`
`600
`
`500
`400
`©
`300
`©
`+
`rs
`200
`iT9) pay o” N
`
`
`
`100
`o
`foo)
`x
`
`0 a
`
`0
`
`2
`
`4
`
`6
`
`8
`
`10
`
`12
`
`14
`
`min]
`
`Customized Report: karlo
`
`Sorted By
`Calib. Data Modified
`Multiplier
`
`: Signal
`: 01/14/2002
`: 1.000000
`
`1:00:30 PM
`
`Signal:
`
`1 DADI C, Sig=210,8 Ref=360,100
`
`Peak
`#
`
`RT
`(min)
`
`Type Width Height
`([min]
`
`Area
`[mAU*s]}
`
`Area
`%
`
`Amount
`mg/ml
`
`Name
`
`3.54 BB
`1
`4.29 PB
`2
`0.00
`3.
`5.88 PB
`4
`6.68 BB
`5
`7.20 PP
`6
`8.34 BB
`7
`9.68 BP
`8
`9 10.88 BB
`10 11.73 BP
`11 13.00 BB
`12 14.28 VB
`
`11.170
`2.15
`0.081
`15.769
`3.05
`0.080
`0.000
`0.00
`0.000
`0.132 2.23e3 1.78624
`0.081
`37.91
`198.693
`0.072
`1.39
`6.156
`0.085 264.54 1423.633
`0.084
`6.80
`36.172
`0.115
`2.13
`16.999
`0.078
`42.61
`213.630
`0.239
`7.86
`127.571
`0.099 356.95 2238.477
`
`0.05
`0.07
`0.00
`80.64
`0.90
`0.03
`6.43
`0.16
`0.08
`0.96
`0.58
`10.11
`
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`
`L-224,715
`
`HPLCO157
`
`01/29/2002
`
`8:59:07 AM
`
`Page 1 of 2
`Merck Exhibit 2129, Page 16
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 16
`Mylan v. Merck, IPR2020-00040
`
`
`
`Data file
`>C: \HPCHEM\HPLCO157\DATA\099-0201.D
`Signal:
`2 DAD] E, Sig=268,16 Ref=360,100
`
`Peak
`#
`
`RT
`{min]
`
`Type Width
`{min}
`
`Height
`
`Area
`
`Area
`
`(mAU*s]
`
`%
`
`Sample Name: 70316-001
`
`0.00
`1
`5.88
`2
`6.68
`3
`8.34
`4
`5 14.28
`
`BB
`BB
`BB
`BB
`
`0.000
`0.078
`0.079
`0.085
`0.099
`
`L-224,715
`
`000000
`.000000
`000000
`.000000
`000000
`
`*** End of Report ***
`
`HPLCO157
`
`01/29/2002
`
`8:59:07 AM
`
`Page 2 of 2
`Merck Exhibit 2129, Page 17
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 17
`Mylan v. Merck, IPR2020-00040
`
`
`
`Data file
`
`:C:\HPCHEM\HPLCO157\DATA\009-0101.D
`
`Sample Name: 70316-001
`
`14.0mg/25ml of isolated besylate salt
`
`->
`
`: 70316-001
`
`: hansen
`
`6:59:40 AM
`
`Seq Line
`
`Vial No
`
`:
`
`:
`
`:
`
`l
`
`9
`
`1
`2 pl
`
`Injection Date : 01/31/2002
`
`oe: Name
`
`Acq Operator
`
`Inj. No.
`Inj. Vol.
`: C:\HPCHEM\HPLCO157\METHODS\715.M
`Method
`: 01/14/2002
`1:00:57 PM
`Last Changed
`75/25 0.1% HC104/Acetonitrile, 1ml/min
`10min 25/75 water/acn; 75/25 from 10 to 14 min
`waters cl8 symmetry, 250 nm
`
`DAD1 C, Sig=210,8 Ref=360,100 (009-0101.D)
`
`4
`2
`DAD1 E, Sig=268,16 Ref=360,100 (009-0101.D)
`
`
`
`Sorted By
`Calib. Data Modified
`Multiplier
`
`: Signal
`: 01/14/2002
`: 1.000000
`
`1:00:30 PM
`
`Signal:
`
`1 DAD1 C, Sig=210,8 Ref=360, 100
`
`Peak
`#
`
`RT
`[min]
`
`Type Width Height
`{min]
`
`Area
`(mAU*s]
`
`Area
`g
`
`Amount
`mg/ml
`
`Name
`
`2.48 VV
`1
`2.59 VB
`2
`5.52 BB
`3
`4 13.24 BP
`
`5.400
`1.70
`0.047
`837.035
`0.089 137.80
`0.082 276.52 1469.249
`0.195
`1.74
`20.490
`
`0.23
`35.89
`63.00
`0.88
`
`0.000000
`0.000000
`0.387022
`0.000000
`
`L-224,715 @4F
`
`Signal:
`
`2 DAD1 E, Sig=268,16 Ref=360,100
`
`Peak
`#
`
`RT
`[min]
`
`Type Width Height
`{min]
`
`Area
`[mAU*s]
`
`Area
`%
`
`Amount
`mg/ml
`
`Name
`
`2.59 BB
`1
`5.52 BB
`2
`3.13.26 PP
`
`0.088
`0.082
`0.215
`
`4.11
`31.93
`1.10
`
`24.614
`169.240
`14.711
`
`11.80
`81.15
`7.05
`
`0.000000
`0.387022
`0.000000
`
`L-224,715
`
`HPLC0157
`
`01/31/2002
`
`7:13:58 AM
`
`Page 1 of 2
`Merck Exhibit 2129, Page 18
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 18
`Mylan v. Merck, IPR2020-00040
`
`
`
`Data file
`
`:C:\HPCHEM\HPLCO157\DATA\010-0101.D
`
`Sample Name: 70316-0011
`
`3.108g/50ml of 16.8g ML 's
`
`Injection Date : 01/31/2002
`Sample Name
`> 70316-0001
`Acq Operator
`: hansen
`
`9:16:19 AM
`
`Seq Line
`Vial No
`Inj. No.
`Inj. Vol:
`: C:\HPCHEM\HPLCO157\METHODS\715.M
`Method
`: 01/14/2002
`1:00:57 PM
`Last Changed
`lml/min
`75/25 0.1% HC104/Acetonitrile,
`75/25 from 10 to 14 min
`10min 25/75 water/acn;
`waters cl8 symmetry, 250 nm
`
`DAD1 C, Sig=210,8 Ref=360,100 (010-0107.D)
`
`
`
`
`
`Sorted By
`Calib. Data Modified
`Multiplier
`
`Signal
`01/14/2002
`1.000000
`
`1:00:30 PM
`
`Signal:
`
`1 DAD C, Sig=210,8 Ref=360,100
`
`Peak
`#
`
`RT
`[min]
`
`Type Width Height
`(min]
`
`Area
`
`[mAU*s]
`
`2.39 VV
`1
`2.49 VV
`2
`2.60 VB
`3
`3.63 BB
`4
`5.05 PB
`5
`5.55 PV
`6
`5.88 VB
`7
`6.76 BB
`8
`7.82 BV
`9
`8.02 VV
`10
`8.33 VV
`11
`8.50 VB
`12
`9.27 VP
`13.
`9.89 BV
`14
`15 10.09 VB
`
`0.058
`0.042
`0.089
`0.082
`0.086
`0.083
`0.078
`0.084
`0.085
`0.092
`0.107
`0.082
`0.100
`0.087
`0.084
`
`NO > wn
`
`wo ~) hw
`
`w
`
`on
`
`oooocoooooo0oo0o0000
`
`. 000000
`000000
`000000
`000000
`000000
`- 124960
`000000
`000000
`. 000000
`000000
`000000
`000000
`000000
`000000
`000000
`
`L-224,715
`
`HPLCO157
`
`01/31/2002
`
`Page 1 of 2
`Merck Exhibit 2129, Page 19
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 19
`Mylan v. Merck, IPR2020-00040
`
`
`
`Data file
`Peak
`#
`
`:C:\HPCHEM\HPLC0O157\DATA\010-0101.D
`RT
`Type Width Height
`Area
`Area
`[min]
`[min]
`[mAU*s]
`%
`
`Amount
`mg/ml
`
`Sample Name: 70316-0011
`Name
`
`16 10.42 BB
`17 12.13 VB
`18 12.93 VB
`
`0.091
`0.092
`0.089
`
`45.48
`4.99
`7.43
`
`269.598
`30.715
`42.450
`
`3.53
`0.40
`0.56
`
`0.000000
`0.000000
`0.000000
`
`Signal:
`
`2 DAD] E, Sig=268,16 Ref=360,100
`
`Peak
`#
`
`RT
`{min]
`
`Type Width Height
`{min]
`
`Area
`{mAU*s]
`
`Area
`%
`
`Amount
`mg/ml
`
`Name
`
`5.05 BB
`1
`5.55 BB
`2
`5.88 BP
`3
`9.27 PP
`4
`5 10.09 PP
`6 10.42 BP
`
`0.087
`0.081
`0.083
`0.098
`0.088
`0.093
`
`1.62
`10.55
`5.50
`1.45
`1.00
`4.53
`
`9.085
`55.201
`29.482
`8.968
`5.712
`27.611
`
`6.68
`40.57
`21.67
`6.59
`4.20
`20.29
`
`0.000000
`0.124960
`0.000000
`0.000000
`0.000000
`0.000000
`
`L-224,715
`
`**x* End of Report ***
`
`HPLCO157
`
`01/31/2002
`
`9:30:35 AM
`
`Page 2 of 2
`Merck Exhibit 2129, Page 20
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 20
`Mylan v. Merck, IPR2020-00040
`
`
`
`Data file
`
`:C:\HPCHEM\HPLCO157\DATA\003-0101.D
`
`Sample Name: 70316-001
`
`hydrog after resubmission more concentrated
`
`->
`
`Injection Date : 01/30/2002
`Sample Name
`: 70316-0011
`Acq Operator
`: hansen
`
`8:54:32 AM
`
`Seq Line
`Vial No
`Inj. No.
`Inj. Vol.
`: C:\HPCHEM\HPLCO157\METHODS\715.M
`Method
`: 01/14/2002
`1:00:57 PM
`Last Changed
`75/25 0.1% HC104/Acetonitrile, 1lml/min
`10min 25/75 water/acn; 75/25 from 10 to 14 min
`waters cl8 symmetry, 250 nm
`
`1
`3
`1
`2 pl
`
`:
`:
`:
`
`DAD1 C, Sig=210,8 Ref=360,100 (003-0101.D)
`
`2
`
`4
`
`DAD1 E, Sig=268,16 Ref=360,100 (003-0101.D)
`
`Sorted By
`Calib. Data Modified
`Multiplier
`
`: Signal
`: 01/14/2002
`: 1.000000
`
`1:00:30 PM
`
`Signal:
`
`1 DADI1 C, Sig=210,8 Ref=360,100
`
`Peak
`#
`
`RT
`[min]
`
`Type Width Height
`[min]
`
`Area
`(mAU*s]
`
`Area
`%
`
`Amount
`mg/ml
`
`Name
`
`2.19 BV
`1
`2.26 VV
`2
`2.39 VV
`3.
`2.56 VB
`4
`2.96 BB
`5
`3.63 PB
`6
`5.04 BV
`7
`5.20 VP
`8
`5.54 BV
`9
`5.87 VB
`10
`6.76 BB
`11
`7.82 BB
`12
`8.50 BB
`13.
`9.89 BV
`14
`15 10.09 VV
`
`14.120
`3.34
`0.061
`5.355
`1.57
`0.052
`101.057
`24.77
`0.062
`13.440
`2.20
`0.091
`56.805
`12.52
`0.069
`171.121
`32.89
`0.081
`47.409
`8.27
`0.089
`12.356
`2.24
`0.082
`0.089 1.32e3 7313.577
`0.078 691.48 3458.091
`0.085
`24.08
`129.711
`0.090
`7.97
`49.417
`0.082
`1.51
`8.044
`0.087
`5.33
`29.603
`0.105
`2.88
`20.953
`
`0.11
`0.04
`0.81
`0.11
`0.45
`1.37
`0.38
`0.10
`58.41
`27.62
`1.04
`0.39
`0.06
`0.24
`0.17
`
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`1.939303
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`
`L-224,715
`
`HPLCO157
`
`01/30/2002
`
`9:08:55 AM
`
`Page 1 of 2
`Merck Exhibit 2129, Page 21
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 21
`Mylan v. Merck, IPR2020-00040
`
`
`
`Data file
`Peak
`#
`
`:C:\HPCHEM\HPLCO157\DATA\003-0101.D
`RT
`Type Width Height
`Area
`Area
`(min)
`(min)
`[mAU*s]
`%
`
`16 10.41 VB
`17 10.89 BP
`18 12.15 PP
`19 12.66 BV
`20 12.92 VV
`21 13.21 VB
`
`38.65
`0.107
`1.29.
`0.104
`1.85
`0.116
`1.31
`0.109
`0.086 140.72
`0.164
`2.18
`
`254.861
`9.002
`14.832
`10.214
`777.889
`23.185
`
`2.04
`0.07
`0.12
`0.08
`6.21
`0.19
`
`Signal:
`
`2 DAD1 E, Sig=268,16 Ref=360,100
`
`Amount
`mg/ml
`
`0.000000
`0.000000
`0.000000
`0.000000
`0.00000G
`0.00000G
`
`Sample Name: 70316-0011
`Name
`
`Peak
`#
`
`RT
`[min]
`
`Type Width Height
`[min]
`
`Area
`{mAU*s]
`
`Area
`%
`
`Amount
`mg/ml
`
`Name
`
`5.04 BB
`1
`5.54 BV
`2
`5.87 VB
`3.
`7.82 BP
`4
`5 10.40 BB
`6 12.92 BB
`7:13.21 BB
`
`2.20
`0.090
`0.083 164.74
`0.085
`8.23
`0.085
`1.15
`0.109
`4.06
`0.089
`2.99
`0.148
`1.04
`
`12.764
`888.075
`45.889
`6.638
`27.613
`17.188
`9.788
`
`1.27
`88.11
`4.55
`0.66
`2.74
`1.71
`0.97
`
`0.000006
`1.939303
`0.000000
`0.000000
`0.000000
`0.000006
`0.00000C
`
`L-224,715
`
`*** End of Report ***
`
`HPLC0157
`
`01/30/2002
`
`9:08:55 AM
`
`Page 2 of 2:
`Merck Exhibit 2129, Page 22
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 22
`Mylan v. Merck, IPR2020-00040
`
`
`
`NO. 1
`
`MLW.
`
`STRUCTURAL FORMULA:
`
`EMPIRICAL FORMULA:
`
`__-_
`
`CATALYST
`SGLVENT
`” MOLES OF HYDROGEN REQUIRED
`OTHER MATERIALS
`
`.
`
`G.
`
`OF
`
`e{ yc
`
`ky et
`
`ML. OF
`~~
`
`G. MOLES
`
`.
`
`2002012956.001
`
`1/29/02
`
`- 1/30/02
`
`200201 2956.00 (
`HYDROGENATIONOR HIGH PRESSURE REACTION
`
`EXT. CSS52
`DATE 2 d ames?
`UESTED BY Hes LA
`AVN AIA
`BLOG/RM
`;
`ole Ge
`noTeBook-paGeNo._/:7!2
`2r~¥
`y ne
`PROJECTNO.ssPROVECT
`CHECK HEREIF REACTION IS GMP/GLP Q
`
`AMOUNT
`
`G. MOLES
`
`motes 22.00/95 Wo:
`NO.1.
`hot # LC IF 2S
`Ale
`S0°T
`OF
`CATALYST.EN CG.
`ML.
`OF
`SOLVENT
`OTHER MATERIALS
`xO m.
`VESSEL SIZE
`EXTERNAL
`REC. POINT INTERNAL —__
`CELL NO____ HEATER NO
`ML.
`SYSTEM VOLUME__7_2-—__
`SHAKER TANK
`Te
`LINER
`SHAKER NO___>. &
`LBS.
`ifs. eh.
`AOLS
`MOLES= 7: 4/
`Les/MoLeE_
`iaes_ee —————————————
`C'D H, PRESSURE DROP =
`DITIONS________ HRS. AT_ZA_ oc. misc. paTA: 4 fase e
`PRESSURE
`
`&8SSESS RUN BY } Asay DATE linn 94 Nand
`
`Ste ott
`
`REACTION CONDITIONS, ETC.
`“
`2
`
`PRECAUTIONS:
`
`BOMB NO.
`AUX. TANK
`
`DROP
`
`T
`
`01:33
`01:48
`02:03
`02:18
`02:33
`02:48
`03:03
`
`MERCK & CO., INC.
`RRALO REV FURR
`
`RUN BY
`
`DATE —
`
`Merck Exhibit 2129, Page 23
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 23
`Mylan v. Merck, IPR2020-00040
`
`
`
`1/29/02
`
`ShkrS6 Pressr
`Shkr56 H2 Uptake
`ShkrS6 Product Temp
`
`9:17.54
`1129/02
`
`13:48:01
`1429102
`
`Hist.FIX.PTS607.F_CV
`Hist.FIXDTS609.F_CV
`Mist.FIX.TES603.F_CV
`
`2002012956.001
`
`Ce
`
`18:18:08
`1129/02
`
`2248-15
`
`Merck Exhibit 2129, Page 24
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 24
`Mylan v. Merck, IPR2020-00040
`
`
`
`2002012856.001
`
`1/28/02
`
`- 1/29/02
`
`Qco2ol Afb-00 |
`HYDROGENATION OR HIGH PRESSURE REACTION
`DUESTED BY Howey siogam—“OVPAUL ite pate2
`PROJECTNO_=2'')ssprovect—_adeMiBForeBo0x-paceno/2=e")
`7
`1 a
`TNA CO
`CHECK HERE IF REACTION IS GMP/GLP O
`ING
`MATERIA’
`
`7
`
`q
`
`NO.1 NO. 2
`
`Mw.2 AMOUNT7.+ G.eMotes_/_sdMW. Ls AMOUNT CG. MOLES
`
`STRUCTURAL FORMULA:
`.
`SN Ae
`;
`LoS ALsa,
`‘ee
`Looky
`
`CATALYST
`sovent
`MOLES OF HYDROGEN REQUIRED
`OTHER MATERIALS
`*
`‘
`‘
`-K\ 4
`REACTION CONDITIONS, ETC.
`Fea
`
`PRECAUTIONS:
`
` TO BE FILLED IN BY HYDROGENATION LABORATORY
`
`noi22 Og CMs 2HOIS noe,—ts MoS
`
`catatyst___—*@JGOOg. of 4 Zed di fH -CYTAS6
`
`yc20)
`SOLVENT ML.
`OOF
`
`
`OTHER MATERIALS
`
`CELL NO.____ HEATERNO.
`REC. POINT INTERNAL ____ EXTERNAL_______ BOMB NO________vessecsize____%0 mt.
`SHAKER NO___24 LINER __________ SHAKER TANK AUX. TANK _______ SYSTEM VOLUME_7% ML.
`CDH, pressure DROP= 79.9 eso20/5 Motes ZY as,
`BNpITIONS________ srs. at_f4+
`oc. misc. paTA:
`“%_- Atm He.
`
`oe|
`
`TIME
`
`TEM
`
`ase DRCPaeeDRoF
`BSSSSESSEZ
`
`EMPIRICAL FORMULA:
` MERCK & CO., INC.
`40
`
`TEMP.
`
`DROP
`
`DDMMDDMDDMDMDDADWDOnN™
`
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`
`R-ASLA REV GAR
`
`RUN BY Uli DATE Vn 25 2a
`RUN BY
`DATE
`
`Merck Exhibit 2129, Page 25
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 25
`Mylan v. Merck, IPR2020-00040
`
`
`
`2002012856.001
`
`ShkrS6 Product Temp
`
`Hist.FIX PT5607.F_CV
`Hist.FiX.OTS609.F_CV
`Hist.FIX.TE5603.F_CV
`
`18:46:38
`1/28/02
`
`Shkr56 Pressr
`Shkr56 H2 Uptake
`
`Merck Exhibit 2129, Page 26
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 26
`Mylan v. Merck, IPR2020-00040
`
`
`
`2002013056.001
`
`1/30/02
`
`- 1/31/02
`
`20040130 56-60 |
`HYDROGENATION OR HIGH PRESSURE REACTION
`DATE wy nan 2092.
`EXT. OSs2
`Foo ck22G 4q
`I
`PROJECT NO_L22T7IS——pRovecT —Mvcoealy NOTEBOOK - PAGE NO._} 9 3te~ 08
`CHECK HERE IF REACTION IS GMP/GLP ©
`—STARTING
`
`NO. 1
`
`«(MOLES
`MLW. 31s AMOUNT _—15O G. moves.5 WwW. AMOUNT CG.
`fa. PAIS
`STRUCTURAL FORMULA:
`cataryst___O./5 ig.
`OF
`SOLVENT a. oF—_AT
`t
`Daav
`MOLES OF HYDROGEN REQUIRED
`yOmeorN
`J Bm
`OTHERMATERIALS
`~~ mm
`:
`-_
`
`. ‘ow,
`
`F
`
`ON
`+
`3
`
`Lot wl wlal THE
`
`REACTION CONDITIONS,ETC.
`oPSa
`,
`
`i
`
`;
`SVC
`
`EMPIRICAL FORMULA:
`
`PRECAUTIONS:
`3
`hi
`2% aN, 2F,
`TO BE FILLED IN BY HYDROGENATION LABORATORY
`
`notFIO ce. mores 20045 no
`CATALYsT____OIG og.
`or LOH
`/,
`—
`SOLVENT. OOF A
`OTHER MATERIALS
`
`CELL NO._____ HEATERNO. REC. POINT INTERNAL _____ EXTERNAL ____s BOMB NOW VESSEL size___0_ML.
`SHAKER NO___944 LINER ____s SHAKER TANK AUX. TANK ___ SYSTEM VOLUME_“72-—_ ML.
`
`C'DH, PRESSURE DROR=—GFDB.tesimore_O-OO/SSMS ZH LBS.
`
`pitions__Jf HRS. AT_~S@ c. MISC. DATA: VO,
`
`MATERIAL_
`
`~~ | DROFeeDROP
`eepeee
`
`TIME
`
`TEMP
`
`00000000000O
`
`Q0000 111tiai
`
`]51
`
`]
`LJ
`
`ff
`
`l
`
`‘oo
`
`1
`
`1]
`Ul
`
`RARLA REV RRR
`MERCK&CO., INC.
`
`RUNBy { WbudsrTe la. Fo atl
`RUN BY
`
`Merck Exhibit 2129, Page 27
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 27
`Mylan v. Merck, IPR2020-00040
`
`
`
`2002013056.001
`
`
`
`8.46'18
`1430/02
`
`13:16:25
`1/30/02
`
`17:46:32
`1/30/02
`
`(30/02
`
`2:46:47
`1/31/02
`
`Shki56 Product Temp
`
`Hist.FIX.PTS607.F_CV
`Hist FIX.DTS609.F_CV
`i
`
`ShkrS6 Pressr
`Shkr56 H2 Uptake
`
`3
`
`Merck Exhibit 2129, Page 28
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 28
`Mylan v. Merck, IPR2020-00040
`
`
`
`
`
`=NNNNNNNNNNRNONORRKDDDNONRNNDRONOND
`
`2002013055.001
`
`1/30/02
`
`HYDROGENATION OR HIGH PRESSURE REACTION
`
`aa
`fo BRET
`H~>¢4
`UESTED BY
`BLDG/RM
`ext. OS5Z
`pate
`_30 dan 2eve
`prosectno._*_2247!5_ provect
`M b00 AAS
`NOTEBOOK- PAGE NO. 2°3(§-0|
`
`CHECK HERE IF REACTION IS GMP/GLP OMATERIAL__—-STARTING
`
`
`2
`
`NO.1
`
`S53 amount 259 sg. motes
`
`AMOUNT
`
`G. MOLES
`
`STRUCTURAL FORMULA:
`
`OF
`G.
`~_
`1a
`CATALYST
`SOLVENT ________-/2_ ML. OF
`“MOLES OF HYDROGEN REQUIRED
`San vel
`OTHER MATERIALS
`
`12 1.PA LC
`fac o(]
`
`REACTION CONDITIONS,ETC.
`So°c HoP+
`
`EMPIRICAL FORMULA: Ci 5 If5\NPy F
`TO BE FILLED IN BY HYDROGENATION LABORATORY
`
`PRECAUTIONS:
`
`NO.2:
`
`G. MOLES
`
`G. motes _2-O0f
`(750
`NO.1:
`Gc. of L2% i
`-fS0
`CATALYST
`SOLVENT.CsCl. 8_CO
`OTHER MATERIALS
`REC. POINT INTERNAL —_____ EXTERNAL
`CELL NO.___ HEATER NO.
`SHAKER NO.LINER SHAKER TANK
`
`BOMB NO
`AUX. TANK
`
`vesset size__— OM.
`SYSTEM VOLUME_S77 ML.
`MOLES= Gy LBS.
`
`C'D H, PRESSURE DROP= 26S issmoue_O- OOS.
`BNDITIONS.___— RS. ATO.
`cc.
`isc. DATA:
`
`‘
`
`a|P
`
`TEMPteeDROP
`
`RESSURE
`
`—c
`—s
`
`TIME
`
`TEMP.
`
`DROP
`
`TIME
`
`TEMP.
`
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`40
`
`TIME
`
`NNNANNRONNONRONOOONONRDORORD
`
`MERCK&CO., INC.
`RASA REV RAR
`
`ry)
`
`RUN BY
`
`RUN BY
`
`/ DATE
`
`DATE
`
`Co
`
`2 20—
`
`Merck Exhibit 2129, Page 29
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 29
`Mylan v. Merck, IPR2020-00040
`
`
`
`2002013055.001
`
`Shk155 Pressr
`ShkrS5 H2 Uptake
`Shkr55 Product Temp
`
`Hist.F1X.PTS507.F_CV
`Hist. FIXDTSS09. F_CV
`ist.FIX.TESSO3.F_CV
`
`Merck Exhibit 2129, Page 30
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 30
`Mylan v. Merck, IPR2020-00040
`
`
`
`Data file
`
`:C:\HPCHEM\HPLCO157\DATA\002-0101.D
`
`Sample Name: 70316-0001
`
`hydrog after resubmission
`
`->
`
`Injection Date : 01/30/2002
`Sample Name
`: 70316-0001
`Acq Operator
`: hansen
`
`8:25:41 AM
`
`Seq Line
`Vial No
`Inj. No.
`Inj. Vol
`: C:\HPCHEM\HPLCO157\METHODS\715.M
`Method
`: 01/14/2002
`1:00:57 PM
`Last Changed
`75/25 0.1% HC104/Acetonitrile, 1ml/min
`10min 25/75 water/acn; 75/25 from 10 to 14 min
`waters cl8 symmetry, 250 nm
`
`:
`:
`:
`
`1
`2
`1
`2 pl
`
`DAD1 C, Sig=210,8 Ref=360,100 (002-0101.D)
`
`DAD1 E, Sig=268,16 Ref=360,100 (002-0101.D)
`
`Sorted By
`Calib. Data Modified
`Multiplier —
`
`> Signal
`: 01/14/2002
`: 1.000000
`
`1:00:30 PM
`
`Signal:
`
`1 DADI C, Sig=210,8 Ref=360,100
`
`Peak
`#
`
`RT
`(min]
`
`Type Width Height
`[min]
`
`Area
`{mAU*s]}
`
`Area
`%
`
`Amount
`mg/ml
`
`Name
`
`2.24 BB
`1
`2.48 BV
`2
`2.99 BB
`3.
`3.54 BB
`4
`5.41 PV
`5
`0.00
`6
`5.80 VB
`7
`6.69 BP
`8
`7.65 BB
`9
`10 10.31 PB
`11 12.88 BB
`12 13.27 BB
`
`9.424
`2.02
`0.070
`17.655
`4.22
`0.065
`11.327
`2.32
`0.075
`32.437
`5.67
`0.089
`0.103 234.39 1553.550
`0.000
`0.00
`0.000
`0.094 116.77
`699.888
`0.096
`4.00
`24.515
`0.113
`1.50
`12.218
`0.119
`6.59
`47.711
`0.089
`27.20
`155.375
`0.132
`1.35
`12.066
`
`0.37
`0.69
`0.44
`1.26
`60.30
`0.00
`27.17
`0.95
`0.47
`1.85
`6.03
`0.47
`
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`0.000000
`
`L-224,715
`
`HPLCO157
`
`01/30/2002
`
`8:40:02 AM
`
`Page 1 of 2
`Merck Exhibit 2129, Page 31
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 31
`Mylan v. Merck, IPR2020-00040
`
`
`
`:C:\HPCHEM\HPLCO157\DATA\002-0101.D
`Data file
`Signal:
`2 DAD] E, Sig=268,16 Ref=360,100
`
`Sample Name: 70316-001
`
`Peak
`#
`
`RT
`[min]
`
`Type Width Height
`{min]
`
`Area
`[mAU*s]
`
`Area
`%
`
`Amount
`mg/ml
`
`Name
`
`1
`2
`3.
`
`5.41 BB
`0.00
`5.80 BB
`
`0.098
`0.000
`0.094
`
`26.83
`0.00
`1.34
`
`165.704
`0.000
`7.981
`
`95.41
`0.00
`4.59
`
`0.000000
`0.000000
`0.000000
`
`L-224,715
`
`*** End of Report ***
`
`HPLCO157
`
`01/30/2002
`
`8:40:02 AM
`
`Page 2 of 2
`Merck Exhibit 2129, Page 32
`Mylan v. Merck, IPR2020-00040
`
`Merck Exhibit 2129, Page 32
`Mylan v. Merck, IPR2020-00040
`
`
`
`
`
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`
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