`E.I. du Pont de Nemours & Co. and
`Acher-Daniels-Midland Co. v. Furanix Technologies BV
`IPR2015-01838
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`1),//E» 0
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`3
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`Ex - eriment
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` :5’ of
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`Experiment: OXE-073
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`/2. May09 ABE
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`R0
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` THE:
`133.19 IEIEEEII
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`8 1-07-2
`s37371or7
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`Table 2: Apparatus
`Apparatus
`Brandi type
`Guard Column
`
`HPLC06
`Agilent
`none
`
`Column
`
`Flow (mVmin)
`Oven temp (°C)
`Mobile phase
`
`Method name
`analyzing
`Apparatus
` III S ’-‘
`
`tirr
`
`Sunfire CI8, 4.6'l0 cm, 3.5 um, pan no.
`186002553
`I .0
`40.0
`Gradient: 0.2% TFA with McOH : ACN
`(50:50)
`0803 I3-Oxe-gradient~35min.met
`
`HTHP (ES
`
`
`
`I051‘
`143
`
` -
`
`
`
`
`
` u
`
`Date weighing. dissolving and adding Cat and substrate
`.
`Date starting reaction ofexperimcnt
`Date weighing. dissolving and adding Saeeharine stock solution :
`Date of analyzing with the HPLC
`o
`HPl..C~analyzing according HPLC-6 logboek
`
`Experimental
`
`.
`..
`Load blocks accordingtablel nu I6. Weighing tolerance '~ 'I‘.I."‘:‘ .:
`
`60
`
`
`
`
`
`Date/W-Is
`
`A r E Add stirring magnet.
`Close with tcflon/rubber cap.
`Bring under pressure with Aj_Ltill §9_flu_at RT
`Placed in preheated HTHP QCS of [59 °c according settings in table 2, during
`Placed immediately afier the reaction time in an ice bath during 35 minutes.
`Open and thereby decompress react rs.
`70 77:4
`Add 1.0 ml of DMSO.
`‘fair
`Add 5.0 ml of Saccharine stock solution. table 5.
`These dilutions where stirred for Iflminutcs.
`
`Table 4: Substrate MMF solutions, in table II to 12 calle
`
`These dilutions to 7 times were transferred to 10 ml vials. - -9.A'r*/1,773 A £3
`Dilutions to 700 times were made by I0 ul ofdilutions 3 times + 990 pl orWater in HPLC vials.
`
`-
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`( MN
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`2
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`Is! %
`name
`concentration
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