Diclazepam the Drug Enforcement Administration's Special Testing and Research Laboratory Generated This Monograph Using Structurally Confirmed Reference Material

Diclazepam The Drug Enforcement Administration's Special Testing and Research Laboratory generated this monograph using structurally confirmed reference material.

3CH N N Cl

1. GENERAL INFORMATION

IUPAC Name: 7-Chloro-5-(2-chlorophenyl)-1-methyl-1,3-dihydro- 2H-1,4-benzodiazepin-2-one

CAS#: 2894-68-0

Synonyms: 2'-Chloro-diazepam, chlorodiazepam, Ro5-3448

Source: 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) 152.2

Base C16H12Cl2N2O 319.19 Not Determined

Latest Revision: 8/25/2017 SWGDRUG.org/monographs.htm Page 1 of 5 Diclazepam 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 ~12 mg/mL in CD3OD containing TMS for 0 ppm reference and dimethylsulfone 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 HNMR: Diclazepam; Lot# RM-161026-03; CD3OD; 400MHz Dimethylsulfone

5 from CD3OD from CD3OD TMS 4

0 16 1 31

7 6 5 4 3 2 1 0

6 1 1 1 3

7.60 7.55 7.50 7.45 7.017.006.99 4.700 4.650 3.950 3.900 3.450 Latest Revision: 8/25/2017 SWGDRUG.org/monographs.htm Page 2 of 5 Diclazepam 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 ~4 mg/mL in CHCl3.

Instrument: Agilent gas chromatograph operated in split mode with MS detector Column: HP-5 MS (or equivalent); 30m x 0.25 mm x 0.25 m Carrier Gas: Helium at 1.5 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 280oC at 12 oC/min 3) Hold final temperature for 9.0 min Injection Parameters: Split Ratio = 25:1, 1 L injected MS Parameters: Mass scan range: 30-550 amu Threshold: 100 Tune file: stune.u Acquisition mode: scan Retention Time: 15.882 min EI Mass Spectrum: Diclazepam; Lot# RM-161026-03 ] 6 318318318318318 318318318318318 318318318318318 318318318 318318318 318 283283283283283 283283283283283 283283283283283 283283283 283283283 283 [x 10 Intensity 1.0 290290290290290 290290290290290 290290290290290 290290290 290290290 290 255255255255255 255255255255255 255255255255255 255255255 255255255 255

0.5 177177177177177 177177177177177 177177177177177 177177177 177177177 177 163163163163163 163163163163163 163163163163163 163163163 163163163 163 125125125125125 125125125125125 125125125125125 125125125 125125125 125 275275275275275 275275275275275 275275275275275 275275275 275275275 275 7575757575 7575757575 7575757575 757575 757575 75 150150150150150 150150150150150 150150150150150 150150150 150150150 150 8989898989 8989898989 8989898989 898989 898989 89 111111111111111 111111111111111 111111111111111 111111111 111111111 239239239239239 239239239239239 239239239239239 111 239239239 239239239 239 137137137137137 137137137137137 137137137137137 137137137 137137137 137 219219219219219 219219219219219 219219219219219 219219219 219219219 219 102102102102102 102102102102102 102102102102102 102102102 102102102 102 268268268268268 268268268268268 268268268268268 268268268 268268268 268 190190190190190 190190190190190 190190190190190 190190190 190190190 190 205205205205205 205205205205205 205205205205205 205205205 205205205 205 6363636363 6363636363 6363636363 636363 636363 63 5151515151 5151515151 5151515151 515151 515151 51 4242424242 4242424242 4242424242 424242 424242 EI+42 302302302302302 302302302302302 302302302302302 302302302 302302302 302

50 100 150 200 250 300 m/z

Latest Revision: 8/25/2017 SWGDRUG.org/monographs.htm Page 3 of 5 Diclazepam 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: 1 Aperture: 150 FTIR ATR (Diamond 1 Bounce): Diclazepam; Lot# RM-161026-03 291429142914291429142914291429142914291429142914291429142914286228622862286228622862286228622862286228622862286228622862 291429142914291429142914286228622862286228622862 2914 2862 305730573057305730573057305730573057305730573057305730573057 305730573057305730573057 3057 297929792979297929792979297929792979297929792979297929792979 297929792979297929792979 2979 %Transmittance 121412141214121412141214121412141214121412141214121412141214 121412141214121412141214 1214 72 108110811081108110811081108110811081108110811081108110811081 108110811081108110811081 1081 945945945945945945945945945945945945945945945 945945945945945945 945 148814881488148814881488148814881488148814881488148814881488 148814881488148814881488 1488 553553553553553553553553553553553553553553553 553553553553553553 553 462462462462462462462462462462462462462462462 462462462462462462 462 113511351135113511351135113511351135113511351135113511351135 113511351135113511351135 1135

56 532532532532532532532532532532532532532532532 532532532532532532 532 831831831831831831831831831831831831831831831 831831831831831831 831 817817817817817817817817817817817817817817817 817817817817817817 48 817 745745745745745745745745745745745745745745745 745745745745745745 40 745 166616661666166616661666166616661666166616661666166616661666 166616661666166616661666 1666

32 3500 3000 2500 2000 1500 Wavenumber (cm-1) %Transmittance 121412141214121412141214121412141214121412141214121412141214 121412141214121412141214 1214 72 108110811081108110811081108110811081108110811081108110811081 108110811081108110811081 1081 945945945945945945945945945945945945945945945 945945945945945945 945 148814881488148814881488148814881488148814881488148814881488 148814881488148814881488 1488 649649649649649649649649649649649649649649649 649649649649649649 649 553553553553553553553553553553553553553553553 553553553553553553 553 482482482482482482482482482482482482482482482 482482482482482482 482 462462462462462462462462462462462462462462462 462462462462462462 462 113511351135113511351135113511351135113511351135113511351135 113511351135113511351135 1135

64 891891891891891891891891891891891891891891891 891891891891891891 891 140114011401140114011401140114011401140114011401140114011401 161816181618161816181618161816181618161816181618161816181618 140114011401140114011401 161816181618161816181618 1401 1618 131813181318131813181318131813181318131813181318131813181318 715715715715715715715715715715715715715715715 131813181318131813181318 715715715715715715 1318 715 56 532532532532532532532532532532532532532532532 532532532532532532 532 831831831831831831831831831831831831831831831 831831831831831831 831 817817817817817817817817817817817817817817817 817817817817817817 48 817 745745745745745745745745745745745745745745745 745745745745745745 40 745 166616661666166616661666166616661666166616661666166616661666 166616661666166616661666 1666

32 1700 1600 1500 1400 1300 1200 1100 1000 900 800 700 Wavenumber (cm-1) Latest Revision: 8/25/2017 SWGDRUG.org/monographs.htm Page 4 of 5 Diclazepam The Drug Enforcement Administration's Special Testing and Research Laboratory generated this monograph using structurally confirmed reference material.

4. ADDITIONAL RESOURCES http://forendex.southernforensic.org/index.php/detail/index/1322Forendex https://en.wikipedia.org/wiki/DiclazepamWikipedia

Moosmann, B.; Bisel, P.; Auwärter, V. Characterization of the designer benzodiazepine diclazepam and preliminary data on its metabolism and pharmacokinetics. Drug Test. Analysis (2014) DOI 10.1002/dta.1628

Latest Revision: 8/25/2017 SWGDRUG.org/monographs.htm Page 5 of 5