Acknowledgement Analytically evaluated sample was kindly … · 2019. 1. 21. · AH-7921...
Transcript of Acknowledgement Analytically evaluated sample was kindly … · 2019. 1. 21. · AH-7921...
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ANALYTICAL REPORT
AH-7921
Acknowledgement
Analytically evaluated sample was kindly provided by the Forensic Science Institute
(FSI) Zurich, Switzerland. NMR analyses were performed in ETH Zürich Institute of
Pharmaceutical Sciences by Dr. Bernhard Pfeiffer and are enclosed in this report by
the permission of Dr. Michael Bovens.
MS and FTIR measurements shown in this report were done in NFL.
mailto:[email protected]
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ANALYTICAL REPORT
AH-7921 (C16H22Cl2N2O)
3,4-dichloro-N-{[1-(dimethylamino)cyclohexyl]methyl}benzamide
Remark – other active cpd. detected: none
Sample ID: 1434-16
Sample description: powder - white
Sample type: collected/Kindly provided by Foresic Science Institute Zurich, Switzerland (NMR
confirmed);
Comments1:
Date of entry: 1/15/2016
Substance identified-
structure2 (base form)
Systematic name: 3,4-dichloro-N-{[1-(dimethylamino)cyclohexyl]methyl}benzamide
Other names:
Formula (per base form) C16H22Cl2N2O
Mw (g/mol) 329,27
Salt form: HCl
StdInChIKey JMZROFPPEXCTST-UHFFFAOYSA-N
Compound Class Opioids
Other active cpd. detected none
Add.info (purity..) app. 98%
1 This report has been produced with the financial support of the P r e v e n t i o n o f a n d f i g h t a g a i n s t c r i m e Programme of the European Union (grant agreement number JUST/2013/ISEC/DRUGS/AG/6413). The contents of this report are the sole responsibility
of the National Forensic Laboratory and can in no way be taken to reflect the views of the European Commission. 2 Created by OPSIN free tool: http://opsin.ch.cam.ac.uk/ DOI: 10.1021/ci100384d
http://opsin.ch.cam.ac.uk/
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Report updates
date comments (explanation)
Supporting information
Analytical technique: applied remarks
GC-MS (EI ionization) + NFL GC-RT (min): 10,31
BP(1): 126; BP(2): 127,BP(3) :173,
FTIR-ATR + direct measurement
GC-IR (condensed phase) + consistent with the one from the FSI Zurich (QM>0.99)
GC-MS (Agilent):
GC-method is RT locked to tetracosane (RT=9.53 min). Injection volume 1 ml and split mode (1:50) . Injector temperature: 280
0C.
Chromatographic separation Column: HP1-MS (100% dimethylpolysiloxane), length 30 m, internal diameter 0.25 mm, film thickens 0.25 mm. Carrier gas He: flow-rate 1.2 ml/min. GC oven program: 170
0C for 1 min, followed by heating up to 293
0C at a rate of
18 0C/min, hold for 6.1 min, than heating at 50
0C/min up to 325
0C and finally 2.8 min isothermal.
MSD source EI = 70 eV. GC-MS transfer line T= 2350C, source and quadropole temperatures 280
0C and 180
0C,
respectively. Scan range m/z scan range: from 50 (40) to 550 amu. FTIR-ATR (Perkin Elmer): scan range 4000-400 cm-1; resolution 4cm-1
GC- (MS)-IR condensed phase (GC-MS (Agilent) & IR (Spectra analyses-Danny) IR scan range 4000 to 700,
resolution 4cm-1 GC-method: Injection volume 1 ml and split mode (1:5) . Injector temperature: 280
0C.
Chromatographic separation Column: HP1-MS (100% dimethylpolysiloxane), length 30 m, internal diameter 0.25 mm, film thickens 0.25 mm. Carrier gas He: flow-rate 1.2 ml/min. GC oven program: 170
0C for 1 min, followed by heating up to 293
0C at a rate of
18 0C/min, hold for 6.1 min, than heating at 50
0C/min up to 325
0C and finally 2.8 min isothermal.
Split MS : IR : (1:9) MSD source EI = 70 eV. GC-MS transfer line T= 235
0C, source and quadropole temperatures 280
0C and 180
0C,
respectively. Scan range m/z scan range: from 50 (40) to 550 amu. IR (condesed phase): IR scan range 4000 to 700, resolution 4cm-1
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FIGURES OF SPECTRA MS (EI)
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FTIR-ATR
IR-Condensed phase
END OF NFL data
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0.51.01.52.02.53.03.54.04.55.05.56.06.57.07.58.08.5f1 (ppm)
67
ddd)13
1.08
6.55
3.27
6.34
2.15
0.96
1.02
1.03
1.00
109
1.10
1.11
1.11
1.12
1.13
1.13
1.14
OOO3
788
7.88
1
2
Cl7
Cl8
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102030405060708090100110120130140150160170180f1 (ppm)
22.3
122
.36
25.8
428
.12
28.2
5
37.4
8
40.5
4
57.9
3
76.8
0 CD
Cl3
77.0
6 CD
Cl3
77.3
1 CD
Cl3
126.
1112
9.30
130.
4513
2.89
134.
6913
5.52
165.
22
1 5
6Cl7
Cl8
9
NH
O11
12
13 17
18N19
CH320
CH321
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1.01.52.02.53.03.54.04.55.05.56.06.57.07.58.0f2 (ppm)
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f1 (
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1.52.02.53.03.54.04.55.05.56.06.57.07.58.0f2 (ppm)
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f1 (
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AH-7921-ID1434-16-rpt1AH-7921_NMR_1H_13C_2D