4-Fluoro-PVP - 4-Fluoro-خ±-PVP,4-fluoro-خ±-2-(1-yrrolidinyl)-valerophenone,p...

download 4-Fluoro-PVP - 4-Fluoro-خ±-PVP,4-fluoro-خ±-2-(1-yrrolidinyl)-valerophenone,p 4-fluoro-خ±-pyrrolidionpentiophenone

If you can't read please download the document

  • date post

    17-Aug-2020
  • Category

    Documents

  • view

    0
  • download

    0

Embed Size (px)

Transcript of 4-Fluoro-PVP - 4-Fluoro-خ±-PVP,4-fluoro-خ±-2-(1-yrrolidinyl)-valerophenone,p...

  • Page 1 of 5SWGDRUG.org/monographs.htmLatest Revision: 03/04/2015

    4-Fluoro-PVP The Drug Enforcement Administration's Special Testing and Research Laboratory

    generated this monograph using structurally confirmed reference material.

    1. GENERAL INFORMATION

    IUPAC Name: 1-(4-fluorophenyl)-2-(pyrrolidin-1-yl)pentan-1-one

    CAS#: 850352-31-7

    Synonyms:

    Source:

    4-Fluoro-α-PVP, 4-fluoro-α-2-(1-pyrrolidinyl)-valerophenone,

    4-fluoro-α-pyrrolidionpentiophenone

    DEA Reference Material Collection

    Appearance: White powder

    UVmax(nm): Not Determined

    2. CHEMICAL AND PHYSICAL DATA

    2.1 CHEMICAL DATA

    Form Chemical Formula Molecular Weight Melting Point (oC)

    Base C15H20FNO 249 Not Determined

    HCl C15H20FNO HCl 285 204.4

    F

    O

    N

    CH3

  • Page 2 of 5SWGDRUG.org/monographs.htmLatest Revision: 03/04/2015

    4-Fluoro-PVP The Drug Enforcement Administration's Special Testing and Research Laboratory

    generated this monograph using structurally confirmed reference material.

    3. QUALITATIVE DATA

    3.1 NUCLEAR MAGNETIC RESONANCE

    Sample Preparation: Dilute analyte to ~5 mg/mL inD2O containing TMS for 0 ppm reference and maleic acid as quantitative internal standard.

    Instrument: 400 MHz NMR spectrometer Parameters: Spectral width: at least containing -3 ppm through 13 ppm

    Pulse angle: 90o

    Delay between pulses: 45 seconds 1H NMR: 4-Fluoro-PVP HCl, Lot 0453912-14, D2O 400MHz

    8 7 6 5 4 3 2 1 0

    0

    1

    2

    3

    4

    5

    6

    7

    8

    9

    10

    326112122

    Maleic Acid

    TSP

    D2O

    1

    7.350

    2

    8.125

    2

    3.75 3.50 3.25

    112

    2.2 2.1 2.0

    6

    1.3 1.2 1.1

    2

    0.850

    3

  • Page 3 of 5SWGDRUG.org/monographs.htmLatest Revision: 03/04/2015

    4-Fluoro-PVP The Drug Enforcement Administration's Special Testing and Research Laboratory

    generated this monograph using structurally confirmed reference material.

    3.2 GAS CHROMATOGRAPHY/MASS SPECTROMETRY

    Sample Preparation: Dilute analyte ~3 mg/mL in Methanol.

    Instrument: Agilent gas chromatograph operated in split mode with MS detector Column: DB-1 MS (or equivalent); 30m x 0.25 mm x 0.25 µm Carrier Gas: Helium at 1 mL/min Temperatures: Injector: 280oC

    MSD transfer line: 280oC MS Source: 230oC MS Quad: 150oC Oven program:

    1) 100oC initial temperature for 1.0 min 2) Ramp to 300oC at 12 oC/min 3) Hold final temperature for 9.0 min

    Injection Parameters: Split Ratio = 20:1, 1 µL injected MS Parameters: Mass scan range: 30-550 amu

    Threshold: 100 Tune file: stune.u Acquisition mode: scan

    Retention Time: 8.837 min EI Mass Spectrum: 4-Fluoro-PVP HCl, Lot 0453912-14

    m/z240220200180160140120100806040

    [x 1

    06 ]

    In te

    ns ity

    0.5

    424242 4242424242 4242424242 4242424242 42424242 5 55555 5555555555 5555555555 5555555555 55555555 696969 6969696969 6969696969 6969696969 69696969 757575 7575757575 7575757575 7575757575 75757575 8 48484 8484848484 8484848484 8484848484 84848484

    959595 9595959595 9595959595 9595959595 95959595

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    [x 1

    04 ]

    In te

    ns ity

    424242 4242424242 4242424242 4242424242 42424242 555555 5555555555 5555555555 5555555555 55555555 696969 6969696969 6969696969 6969696969 69696969 757575 7575757575 7575757575 7575757575 75757575 848484 8484848484 8484848484 8484848484 84848484 959595 9595959595 9595959595 9595959595 95959595 10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    10 9

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    12 6

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    13 3

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    16 4

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    17 8

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    18 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    20 6

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    23 2

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

    24 8

  • Page 4 of 5SWGDRUG.org/monographs.htmLatest Revision: 03/04/2015

    4-Fluoro-PVP The Drug Enforcement Administration's Special Testing and Research Laboratory

    generated this monograph using structurally confirmed reference material.

    3.3 INFRARED SPECTROSCOPY (FTIR)

    Insrument: FTIR with diamond ATR attachment (1 bounce) Scan Parameters: Number of scans: 32

    Number of background scans: 32 Resolution: 4 cm-1

    Sample gain: 8 Aperture: 150

    FTIR ATR (Diamond, 1 Bounce): 4-Fluoro-PVP HCl, Lot 0453912-14

    Wavenumber (cm-1)3500 3000 2500 2000 1500

    % Tr

    an sm

    itt an

    ce

    30

    40

    50

    60

    70

    507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507 507

    544 544 544 544 544 544 544 544 544 544 544 544 544 544 544 544 544 544 544 544 544 544577

    577 577 577 577 577 577 577 577 577 577 577 577 577 577 577 577 577 577 577 577 577

    590 59