Succinate → 4-(4-(Oxetan-3-yl)piperazin-1-yl)aniline
Reaction equation
C([O-])(=O)CCC([O-])=O.C(O)(=O)CCC(O)=O.NC1N=C(C2N=C([NH:33][C:34]3[CH:39]=[CH:38][C:37]([N:40]4[CH2:45][CH2:44][N:43]([CH:46]5[CH2:49][O:48][CH2:47]5)[CH2:42][CH2:41]4)=[CH:36][CH:35]=3)C3N(C=CN=3)C=2)C=NC=1.[Al]>[Cu]>[O:48]1[CH2:49][CH:46]([N:43]2[CH2:42][CH2:41][N:40]([C:37]3[CH:38]=[CH:39][C:34]([NH2:33])=[CH:35][CH:36]=3)[CH2:45][CH2:44]2)[CH2:47]1Participants
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Procedure
X-ray powder diffraction (XRPD) analysis of the monomesylate (MSA) and succinate forms of the compound of Example 2 herein were conducted on a diffractometer (PANanalytical XPERT-PRO, PANalytical B.V., Almelo, Netherlands) using copper radiation (Cu Kα, λ=1.5418 Å). Samples were prepared for analysis by depositing the powdered sample in the center of an aluminum holder equipped with a zero background plate. The generator was operated at a voltage of 45 kV and amperage of 40 mA. Slits used were Soller 0.02 rad., antiscatter 1.0°, and divergence. The sample rotation speed was 2 sec. Scans were performed from 2 to 40° 2-theta. Data analysis was performed by X'Pert Highscore version 2.2c (PANalytical B.V., Almelo, Netherlands) and X'Pert data viewer version 1.2d (PANalytical B.V., Almelo, Netherlands). The XRPD patterns for Mono MSA Forms I & II were obtained using the instrument setting as follows: 45 KV, 40 mA, Cu Kα, λ=1.5418 Å, scan range 2.-40°, step size 0.0167°, counting time: 15.875 s. The XRPD patterns for Succinate Forms I & II were obtained using the instrument setting as follows: 45 KV, 40 mA, Cu Kα, λ=1.5418 Å, scan range 2.-40°, step size 0.0084°, counting time: 95.250 s.
Workup
- customSamples were prepared for analysis
- customequipped with a zero background plate
- customantiscatter 1.0°, and divergence
- customwere performed from 2 to 40°
Sources & evidence
- ORD record
- ord-630db7288b7f433190bc44e1af92585e
- Source dataset
- uspto-grants-2016_03
- Patent number
- US09290505B2
Reaction notes
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