L—000224715—006F017
`
`
`
`
`
`17—J‘UN—2002X
`
`
`WHITE
`POWDER
`
`Morphology
`Agglomeration
`
`.
`Observatxcns
`
`2.78 sq. m/g
`
`Empirical Formula:C16H16E‘6N50 408.329 H204? 96.987
`
`
`
` Molecular Weight: 505.317
`
`Project Code' 0431
`
`
`(2R)—4-OXO—4-[3-(TRIFLUOROMETHYL)-5, 6-
`hemlcal name:
`
`
`
`IDIHYDRO [ 1, 2, 4 ] TRIAZOLOH , 3-A] PYRAZIN-7 (8H) -‘{L] -1- (Z, 4 , 5-
`KARL HANSEN
`Prepared By:
`RI FLUOROPHENYL) BUTAN-Z-AMINE PHOSPHORIC ACID SALT
`
`
`
`
`
`Amount Made:
`4.44 KG
`Reference:
`72471-049
`
`Date Of Manufacture:
`05-JUN-2002
`
`
`Sample ID(s):
`200004693
`
`
`Structure:
`
`
`
`ll-JUN-ZOOZ
`Date (5) Tested:
`
`
`
`
`
`Milled:
`N
`Process Change:
`N
`
`Nature Of Change:
`Restricted Release By:
`ARMSTRONG, TILLYER
`
`
` Send To: 5. Martell man-10 1.4 Kg Ph I
`
`
`
`
`
`2.9 Kg Ph 11 a. Martell wen—1o
`
`
`
`
`
`
`Reserve Sample
`RYZE X 1 gram
`
`
`
`
`\ l f - Jay-4471'
`‘
`
`
`arning:
`REFRIGERATED
`PE—ECL CODE
`Storage Conditions :
`
`
`
`
`SODMG FREEZER ’
`
`\ /f'duv—M}
`MICROSCOPIC EXAM
`DISC
`
`
`’5’)”
`CLEAN
`Phase
`ANISOTROPIC
`5°1vent
`DI WATER
`
`
`C
`
`
`Form
`x-RAY
`
`
`
`
`gYSTMLINE’ SAME SURFACE AREA
`
`
`
`
`PREVIOUS(200004568 Surface area
`
`
`
`MURI TY PROFILE
`’
`PARTICLE SIZE
`
`
`
`0 20 g
`Technique.
`RRT 0'95
`
`
`
`RM 0.97
`0'26 %
`Distributin type
`
`
`Total Impurities
`0.46 %
`:Vzrag: s ~e
`
`
`# of quantifiable
`0
`distribution
`
`
`impuritxes <0.10%
`95g <
`0.05 g
`:2 other Impurity
`g < size
`
`
`TITRATION - PERCHLORIC ACID
`Size
`
`
`Analyte
`L—224715-006F
`BULK DENSITY
`
`
`Result
`1002 (“finga
`Loose density
`
`
`TITRATION — SODIUM HYDROXIDE
`Tapped density
`
`
`malyte
`PHOSPHATE
`COLOR (SOLID)
`
`
`
`
`R
`t
`19.4 (w/w)%"
`“he":
`
`
`SORBANCE _ 15-1.
`Concentration
`
`
`LENGTH
`Wavelength
`
`
`
`DI WATER
`Solvent
`M x 100°
`
`
`257.0 nm
`Wavelength 1
`NEPHELOS
`
`
`
`
`37_-, 33¢.
`AB @ wavelength 1
`Solvent
`
`
`KARL FISCHER (KF)
`Concentration
`
`
`Water
`0.3 w/w%
`Result
`RESIDUAL SOLVENTS
`PH
`
`
`(w/w)%
`N.D.
`Eto"
`RESIDUE 0N IGNITION B! ICP
`
`
`PURITY
`"'18 of residue
`<0.05 (w/w)%
`P
`.
`99.5 a
`“My
`CHIRAL PURIT!
`
`
`
`100.00 %
`BASED ON HPLC AREA
`Ratif’mle
`L—224715t
` PERCENT
`
`' Dry basis
`
`'hosphate theory = 19.4%
`
` Iept. Approval:
`13-JUN-2002
`
`
`2.0 grams
`(sample)
`Net wt.
`PLATE LIKE
`< STD 1
`Visual Comparison
`MOSTLY PRIMARY
`PARTICLES AND SOME ‘0 Std
`AGGLOMERATION
`IDENTITY BY FTIR
`Conforms
`YES
`SPECIFIC ROTATION (SOLID)
`Solvent
`D1 WATER
`Concentration
`1.0 (w/v)%
`Specxfic Rotation
`45.6 degrees‘
`DSC CHARACTERIZATION
`T onset 1
`216‘1 degrees -C
`T max 1
`218.2 degrees -C
`Delta H 1
`93,0 J/q
`TG
`N'D‘ W“
`weight Loss 1
`2211 degrees '5
`Final Temp
`HEAVY METALS BY ICP/Ms
`Sigfiiiidafiefigfits
`<10' ppm
`ELEMENTAL ANALYSIS
`Palladium (Pd)
`<3_ ppm
`Copper
`(Cu)
`(3. ppm
`Ruthemum (Ru)
`<3. ppm
`POTENCY AS-IS
`Potency
`As
`
`MICRO TRAC
`VOLUME
`62. um
`38. um
`139_ um
`20- 3
`25 um
`
`0.34 g/mL
`0-53 g/mL
`
`W "ATER
`1.0 (w/v)%
`440 nm
`3-
`
`DI WATER
`1.0 (w/v)%
`0.8 ntu
`
`“1““
`C°ncenmt1°n
`Sample PH
`
`M WATER
`1.0 (w/v):
`4.6 pH
`
`Rationale
`
`99.2 %
`L—224715-006E‘
`PHOSPHATE SALT
`uno-cc-xmx o.o1
`[loo-TOTAL
`IMPURITIES (LCAP
`mama.”
`
`
`
`
`
`Lot Id: 700000942
`
`
`
`
`C. Egan RY818——,B204 Eiserle RY 818— C221, {Thomas RY818——C2,08 Wyvratt RY818-B201,
`
`Restricted
`
`Hansen RY800—B269, Armstrong RY800—D371, Kumke RY819—405 Iflz’J/flle fjififlféé”
`
`R 9 Confidential
`limited 306655
`D DELIVERY SHEET: CH
`ICAL FOR CLINICAL OR P:E2JNICAL TESTING
`Locwifpumo
`wacnso AZ ssm. mm.”
`
`Merck Exhibit 2136 f
`Mylan v. Merck, |PR2020-00040
`
`Merck Exhibit 2136
`Mylan v. Merck, IPR2020-00040
`
`