alpha-PBP Latest Revision: May 16, 2013

CH3

1. GENERAL INFORMATION

IUPAC Name: 1-phenyl-2-(pyrrolidin-1-yl)butan-1-one

CFR: Not Scheduled (5/2013)

CAS#: 13415-54-8 (HCl)

Synonyms: α−Pyrrolidinobutiophenone, α-Pyrrolidinobutyrophenone

Source: DEA Reference Material Collection

Appearance: White powder (HCl)

Kovat's Index: Pending

UVmax (nm): 253.0

2. CHEMICAL AND PHYSICAL DATA

2.1 CHEMICAL DATA

Form Chemical Formula Molecular Weight Melting Point ( oC)
Base C14H19NO 217 Not Determined
HCl C14H19NO . HCl 253 193.4

3. ADDITIONAL RESOURCES

Forendex
http://forendex.southernforensic.org/index.php/detail/index/1163

Wikipedia
http://en.wikipedia.org/wiki/alpha-Pyrrolidinobutiophenone

Page 1 of 4
4. QUALITATIVE DATA

4.1 NUCLEAR MAGNETIC RESONANCE

Method NMR D2O

Sample Preparation: Dilute analyte to ~10 mg/mL in D 2O containing TSP 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
1
H NMR: α-PBP HCl; Lot ALB 225-2; D2O; 400 MHz
Maleic acid (ISTD) HDO

10

TSP
8

2 1 2 1 2 1 1 6 3

8 7 6 5 4 3 2 1 0
Chemical Shift (ppm)
10.0
4 1.5 7.5
3
1.0 5.0
2
1 0.5 2.5

2 1 2 1 2 1 1 6 3

8.00 7.75 5.3005.250 3.75 3.35 3.075 2.2 2.1 2.0 0.825
Chemical Shift (ppm) Chemica... Chemical... Chemi... Chemi... Chemical Shift (ppm) Chemic...

Page 2 of 4
4.2 Gas Chromatography/Mass Spectrometry

Sample Preparation: Dilute analyte ~ 1 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: 230 oC
MS Quad: 150oC
Oven program:
1) 100oC initial temperature for 1.0 min
2) Ramp to 300 oC 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: 9.483 min
EI Mass Spectrum: α-PBP HCl; Lot ALB-225-2
112

1500000
Intensity

1200000

900000

600000
77

113
105
70
41

55
42
51

188
160
128
131

186

300000
146

170

199
202

216
96
58

91

40 60 80 100 120 140 160 180 200 220

m/z
105
112
113
41
42
51
55
58

70
77

91
96
Intensity

188

16000
160
128
131

186
146

170

216
202
199

8000

40 60 80 100 120 140 160 180 200 220

m/z
Page 3 of 4
4.3 INFRARED SPECTROSCOPY (FTIR)

Insrument: FTIR with diamond ATR attachment (3 bounce)

Scan Parameters: Number of scans: 32
Number of background scans: 32
Resolution: 4 cm-1
Sample gain: 8
Aperture: 150

FTIR ATR (Diamond, 3 bounce): α-PBP HCl; Lot ALB 225-2

96

88

2461
2939

80

424
2625
2607

825

661

417
2578

914
1464

1034
%Transmittance

1597
72

1140

588
1448
1354
64

1257

966

690
56

775
1228
48 1684

40

708
3500 3000 2500 2000 1500 1000 500
Wavenumber (cm-1)

96

88
889

505
1161

939

860

80
1001

424
615
825

661

417
1078

914
1304
1464

1034
%Transmittance

1597

1336

72
1140

588
1389
1448

1354

64
1257

966

690

56
775
1228

48
1684

40
708

1700 1600 1500 1400 1300 1200 1100 1000 900 800 700 600 500 400
Wavenumber (cm-1)

Page 4 of 4