4-Bromo-a-PVP - SWGDRUG · 2016. 4. 20. · EI4-Bromo-α-PVP HCl; Lot# Mass RM-160316-01 Spectrum:...

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4-Bromo- a-PVP The Drug Enforcement Administration's Special Testing and Research Laboratory generated this monograph using structurally confirmed reference material. Latest Revision: 3/24/2016 Page 1 of 5 SWGDRUG.org/monographs.htm 1. GENERAL INFORMATION IUPAC Name: 1-(4-bromophenyl)-2-(pyrrolidin-1-yl)pentan-1-one CAS#: NA Synonyms: 4-Bromo-alpha-PVP Source: DEA Reference Material Collection Appearance: Off-white powder (HCl) UV max (nm): Not determined 2. CHEMICAL AND PHYSICAL DATA 2.1 CHEMICAL DATA O N Br CH 3 Form Chemical Formula Molecular Weight Melting Point ( o C) Base C 15 H 20 BrNO 310 Not Determined HCl C 15 H 20 BrNO HCl 346 209.1

Transcript of 4-Bromo-a-PVP - SWGDRUG · 2016. 4. 20. · EI4-Bromo-α-PVP HCl; Lot# Mass RM-160316-01 Spectrum:...

Page 1: 4-Bromo-a-PVP - SWGDRUG · 2016. 4. 20. · EI4-Bromo-α-PVP HCl; Lot# Mass RM-160316-01 Spectrum: 40 60 80 100 120 140 160 180 200 220 240 260 280 300 m/z [x 10 6] Intensity 2 4

4-Bromo-α-PVPThe Drug Enforcement Administration's Special Testing and Research Laboratory

generated this monograph using structurally confirmed reference material.

Latest Revision: 3/24/2016 Page 1 of 5SWGDRUG.org/monographs.htm

1. GENERAL INFORMATION

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

CAS#: NA

Synonyms: 4-Bromo-alpha-PVP

Source: DEA Reference Material Collection

Appearance: Off-white powder (HCl)

UVmax(nm): Not determined

2. CHEMICAL AND PHYSICAL DATA

2.1 CHEMICAL DATA

O

N

Br

CH3

Form Chemical Formula Molecular Weight Melting Point (oC)

Base C15H20BrNO 310 Not Determined

HCl C15H20BrNO HCl 346 209.1

Page 2: 4-Bromo-a-PVP - SWGDRUG · 2016. 4. 20. · EI4-Bromo-α-PVP HCl; Lot# Mass RM-160316-01 Spectrum: 40 60 80 100 120 140 160 180 200 220 240 260 280 300 m/z [x 10 6] Intensity 2 4

4-Bromo-α-PVPThe Drug Enforcement Administration's Special Testing and Research Laboratory

generated this monograph using structurally confirmed reference material.

Latest Revision: 3/24/2016 Page 2 of 5SWGDRUG.org/monographs.htm

3. QUALITATIVE DATA

3.1 NUCLEAR MAGNETIC RESONANCE

Sample Preparation: Dilute analyte to ~12 mg/mL inD2O containing TSP for 0 ppm reference and maleicacid as quantitative internal standard.

Instrument: 400 MHz NMR spectrometerParameters: Spectral width: at least containing -3 ppm through 13 ppm Pulse angle: 90o

Delay between pulses: 45 seconds

1HNMR: 4-Bromo-α-PVP HCl; Lot# RM-160316-01; D2O; 400MHz

8.0 7.5 7.0 6.5 6.0 5.5 5.0 4.5 4.0 3.5 3.0 2.5 2.0 1.5 1.0 0.5 0

326112122

7.907.857.80

22

5.250

1

3.75 3.50 3.25

112

2.2 2.1 2.0

6

1.3 1.2 1.1

2

0.825

3

maleic acid HDO

TSP

Page 3: 4-Bromo-a-PVP - SWGDRUG · 2016. 4. 20. · EI4-Bromo-α-PVP HCl; Lot# Mass RM-160316-01 Spectrum: 40 60 80 100 120 140 160 180 200 220 240 260 280 300 m/z [x 10 6] Intensity 2 4

4-Bromo-α-PVPThe Drug Enforcement Administration's Special Testing and Research Laboratory

generated this monograph using structurally confirmed reference material.

Latest Revision: 3/24/2016 Page 3 of 5SWGDRUG.org/monographs.htm

3.2 GAS CHROMATOGRAPHY/MASS SPECTROMETRY

Sample Preparation: Dilute analyte ~4 mg/mL in CHCl3 base extracted with NaOH

Instrument: Agilent gas chromatograph operated in split mode with MS detectorColumn: HP-5 MS (or equivalent); 30m x 0.25 mm x 0.25 µmCarrier Gas: Helium at 1.5 mL/minTemperatures: 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 280oC at 12 oC/min 3) Hold final temperature for 9.0 minInjection Parameters: Split Ratio = 25:1, 1 µL injectedMS Parameters: Mass scan range: 30-550 amu Threshold: 150 Tune file: stune.u Acquisition mode: scanRetention Time: 12.027 min

EI Mass Spectrum: 4-Bromo-α-PVP HCl; Lot# RM-160316-01

m/z300280260240220200180160140120100806040

[x 1

06 ]In

tens

ity

2

4

3939393939393939393939393939393939393939393941414141414141414141414141414141414141414141 42424242424242424242424242424242424242424242

5454545454545454545454545454545454545454545455555555555555555555555555555555555555555555

56565656565656565656565656565656565656565656

686868686868686868686868686868686868686868686969696969696969696969696969696969696969696975757575757575757575757575757575757575757575

7676767676767676767676767676767676767676767684848484848484848484848484848484848484848484

96969696969696969696969696969696969696969696 9797979797979797979797979797979797979797979798989898989898989898989898989898989898989898124124124124124124124124124124124124124124124124124124124124124124

126126126126126126126126126126126126126126126126126126126126126126

127127127127127127127127127127127127127127127127127127127127127127155155155155155155155155155155155155155155155155155155155155155155 157157157157157157157157157157157157157157157157157157157157157157

183183183183183183183183183183183183183183183183183183183183183183 185185185185185185185185185185185185185185185185185185185185185185EI+

m/z300280260240220200180160140120100806040

[x 1

05 ]In

tens

ity

1

2

3

4

39393939393939393939393939393939393939393939

41414141414141414141414141414141414141414141

42424242424242424242424242424242424242424242

54545454545454545454545454545454545454545454

55555555555555555555555555555555555555555555

5656565656565656565656565656565656565656565668686868686868686868686868686868686868686868

696969696969696969696969696969696969696969697575757575757575757575757575757575757575757576767676767676767676767676767676767676767676

8484848484848484848484848484848484848484848496969696969696969696969696969696969696969696

97979797979797979797979797979797979797979797

98989898989898989898989898989898989898989898103103103103103103103103103103103103103103103103103103103103103103104104104104104104104104104104104104104104104104104104104104104104

124124124124124124124124124124124124124124124124124124124124124124

126126126126126126126126126126126126126126126126126126126126126126 127127127127127127127127127127127127127127127127127127127127127127

128128128128128128128128128128128128128128128128128128128128128128129129129129129129129129129129129129129129129129129129129129129129131131131131131131131131131131131131131131131131131131131131131131132132132132132132132132132132132132132132132132132132132132132132

155155155155155155155155155155155155155155155155155155155155155155 157157157157157157157157157157157157157157157157157157157157157157

158158158158158158158158158158158158158158158158158158158158158158

183183183183183183183183183183183183183183183183183183183183183183 185185185185185185185185185185185185185185185185185185185185185185

186186186186186186186186186186186186186186186186186186186186186186 266266266266266266266266266266266266266266266266266266266266266266 268268268268268268268268268268268268268268268268268268268268268268EI+308 310

Page 4: 4-Bromo-a-PVP - SWGDRUG · 2016. 4. 20. · EI4-Bromo-α-PVP HCl; Lot# Mass RM-160316-01 Spectrum: 40 60 80 100 120 140 160 180 200 220 240 260 280 300 m/z [x 10 6] Intensity 2 4

4-Bromo-α-PVPThe Drug Enforcement Administration's Special Testing and Research Laboratory

generated this monograph using structurally confirmed reference material.

Latest Revision: 3/24/2016 Page 4 of 5SWGDRUG.org/monographs.htm

Wavenumber (cm-1)4000 3500 3000 2500 2000 1500 1000

%Tr

ansm

ittan

ce

50

55

60

65

70

75 449449449449449449449449449449449449449449449449449449449449449449

469469469469469469469469469469469469469469469469469469469469469469

538538538538538538538538538538538538538538538538538538538538538538

580580580580580580580580580580580580580580580580580580580580580580

622622622622622622622622622622622622622622622622622622622622622622

730730730730730730730730730730730730730730730730730730730730730730

749749749749749749749749749749749749749749749749749749749749749749

809809809809809809809809809809809809809809809809809809809809809809

840840840840840840840840840840840840840840840840840840840840840840

866866866866866866866866866866866866866866866866866866866866866866

895895895895895895895895895895895895895895895895895895895895895895

951951951951951951951951951951951951951951951951951951951951951951

10031003100310031003100310031003100310031003100310031003100310031003100310031003100310031068

106810681068106810681068106810681068106810681068106810681068106810681068106810681068

1135113511351135113511351135113511351135113511351135113511351135113511351135113511351135

1183118311831183118311831183118311831183118311831183118311831183118311831183118311831183

1228122812281228122812281228122812281228122812281228122812281228122812281228122812281228

133813381338133813381338133813381338133813381338133813381338133813381338133813381338133813911391139113911391139113911391139113911391139113911391139113911391139113911391139113911441

144114411441144114411441144114411441144114411441144114411441144114411441144114411441

1487148714871487148714871487148714871487148714871487148714871487148714871487148714871487

1579157915791579157915791579157915791579157915791579157915791579157915791579157915791579

1682168216821682168216821682168216821682168216821682168216821682168216821682168216821682

28722872287228722872287228722872287228722872287228722872287228722872287228722872287228722965

296529652965296529652965296529652965296529652965296529652965296529652965296529652965

Wavenumber (cm-1)1760 1680 1600 1520 1440 1360 1280 1200 1120 1040 960 880 800 720 640

%Tr

ansm

ittan

ce

50

55

60

65

70

75 449449449449449449449449449449449449449449449449449449449449449449

469469469469469469469469469469469469469469469469469469469469469469

508508508508508508508508508508508508508508508508508508508508508508

538538538538538538538538538538538538538538538538538538538538538538

580580580580580580580580580580580580580580580580580580580580580580

622622622622622622622622622622622622622622622622622622622622622622

678678678678678678678678678678678678678678678678678678678678678678700700700700700700700700700700700700700700700700700700700700700700

730730730730730730730730730730730730730730730730730730730730730730

749749749749749749749749749749749749749749749749749749749749749749

784784784784784784784784784784784784784784784784784784784784784784809809809809809809809809809809809809809809809809809809809809809809

840840840840840840840840840840840840840840840840840840840840840840

866866866866866866866866866866866866866866866866866866866866866866

895895895895895895895895895895895895895895895895895895895895895895914914914914914914914914914914914914914914914914914914914914914914

951951951951951951951951951951951951951951951951951951951951951951

974974974974974974974974974974974974974974974974974974974974974974

1003100310031003100310031003100310031003100310031003100310031003100310031003100310031003

1039103910391039103910391039103910391039103910391039103910391039103910391039103910391039

1068106810681068106810681068106810681068106810681068106810681068106810681068106810681068

1105110511051105110511051105110511051105110511051105110511051105110511051105110511051105

1135113511351135113511351135113511351135113511351135113511351135113511351135113511351135

1183118311831183118311831183118311831183118311831183118311831183118311831183118311831183

1228122812281228122812281228122812281228122812281228122812281228122812281228122812281228

1282128212821282128212821282128212821282128212821282128212821282128212821282128212821282

1338133813381338133813381338133813381338133813381338133813381338133813381338133813381338

1391139113911391139113911391139113911391139113911391139113911391139113911391139113911391

1441144114411441144114411441144114411441144114411441144114411441144114411441144114411441

1487148714871487148714871487148714871487148714871487148714871487148714871487148714871487

1579157915791579157915791579157915791579157915791579157915791579157915791579157915791579

1682168216821682168216821682168216821682168216821682168216821682168216821682168216821682

3.3 INFRARED SPECTROSCOPY (FTIR)

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

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

Sample gain: 1Aperture: 150

FTIR ATR (Diamond 1 Bounce): 4-Bromo-α-PVP HCl; Lot# RM-160316-01

Page 5: 4-Bromo-a-PVP - SWGDRUG · 2016. 4. 20. · EI4-Bromo-α-PVP HCl; Lot# Mass RM-160316-01 Spectrum: 40 60 80 100 120 140 160 180 200 220 240 260 280 300 m/z [x 10 6] Intensity 2 4

4-Bromo-α-PVPThe Drug Enforcement Administration's Special Testing and Research Laboratory

generated this monograph using structurally confirmed reference material.

Latest Revision: 3/24/2016 Page 5 of 5SWGDRUG.org/monographs.htm

4. ADDITIONAL RESOURCES

No additional resources as of 03/2016