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

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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. O HC3 N N Cl 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 10 9 8 7 6 5 from CD3OD from CD3OD TMS 4 3 2 1 0 6 1 1 1 3 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 Temperatures: Carrier Latest Revision: Latest Retention MS Injection Parameters: Column: Instrument: Sample Preparation: 3.2 42 42 42 420.5 42 1.0 42 42 42 42 42 6 GAS 51 51 51 51 51 Intensity [x 10 ] Parameters: 42 42 42 EI+ 63 63 63 63 63 Gas: 51 51 51 CHROMATOGRAPHY/MASS 42 Time: 50 75 75 75 75 75 5163 63 63 The Drug 1028975 89 102 75 89 75 102 89 89102 102 generated thismonographusingstructurally 8/25/ 63 111 111 111 111 111 8975 89 89 Dilute EnforcementAdministration'sSpecial 2017 102125 102 125 102 125 125 125 11189 111 111 100 137 137 137 137 137 EI MassSpectrum:Diclazepam; 137 137 137 137 137 analyte ~4 mg/mL inCHCl ~4mg/mL analyte 102 125 125 125 150 150 150 150 150 111 137 137 137 163 163 163 163 163 SWGDRUG.org/monographs.htm MS Injector: Helium Oven MS MSD 15.882 Acquisition Tune Threshold: Split HP-5 Agilent 125 Mass 150 150 150 177 177 177 177 177 Quad: Source: Ratio=25:1,1 137 file: MS(or scanrange: program: transferline: SPECTROMETRY 150 163 163 163 min 3) 2) 1) 100 at gas 190150 190 190 190 190 280 Diclazepam stune.u 1.5 Hold Ramp 150 177 177 177 100 177 177 177 chromatographoperatedinsplit mode: 230 equivalent);30m 205 205 205 205 205 o 205163 205 205 205 205 mL/min o C C final 190 190 190 o to C initialtemperature o 30-550 219177 219 219 219 219 C scan 280 280 3 . 205 205 205 temperature L injected 190 Lot# 200 o Testing o C confirmed 219239 219 239 219 239 239 239 C amu 205 at RM-161026-03 12 255 255 255 255 255 x 239 239 239 and 219239 239 239 o 0.25 C/min 268 268 268 268 268 for reference for ResearchLaboratory 275 275 275255 275 255 275 255 9.0 mm 239 283 283 283 283 283 1.0 250 268 268 268 290 290 290 290 290 min x 275 275 275 min mode 275 275 275255 0.25 302 302 302 302 302 283 283 283 material. 268 290 290 290 with 275 318 318 318 318 318 m 302 302 302 283 290 MS 300 318 318 318 detector Page 3of5 302 318 m/z 462 532 553 462 482 462715 462 462 745 532 532 532 532 Page 4 of 5 553 553817 553 553462 462 462 891 831 482 482 482 945462715 462 715 462 715 462 462 745 745 745 532 532 532 532 532 532 532 532 553 553 553 Wavenumber (cm-1) 553 553 553 1081553 553817 553 817 553 817 553 649462 462 462 462Wavenumber (cm-1) 462 1135891831 891 831 891 831 482 482 482 482 482 945715 945 715 945 715 715 715 1214 745 745 745 745 745 715 532 532 532700 532 532 649553 649 553 649 553 553 553 material. 1318 817 817 817 817 817 745 1081891 1081831 891 8311081 891 831 891 831 891 831 9451401 945 945 945 945 715 715 715 800 14881135 1135 1135 715 715817 715 1214 1214 1214 649 649 649745 649 745 649 745 1214 1214 1214 1500 831 Research Laboratory 1618 RM-161026-03 1318 1318 1318 reference 1318 1318 1318 891 1081 1081 10811666 1081 1081 715 715 715 715 715 1401 1401 1401 817 817 817900 and 745 745 745 745 745 14881135 1488 1135 1488 1135 1135 1135 945 831 831 831 Lot# bounce) 1214 1214 1214 1214 1214 891 891 891 (1 891 891 891 16181318 1618 1318 1618 1318 1318 1318 817 817 817 817 817 1666 1666 1666 1000 confirmed 831 831 831 831 831 Testing 945 945831 945 831 831 831 831 1401 1401 14012000 1401 1401 945 945 945 32 1488 1488 1488 1488 1488 1081891 891 891 891 891 1618 1618 1618 1618 1618 9451135 945 945 945 9451100 attachment 1666 1666 1666 1666 1666 1666 1666 1666 1666 1666 scans: 1081 1081 1081 ATR 1214 1200 Diclazepam 32 2500 -1 1135 1135 1135 Bounce): Diclazepam; cm 1 1 4 1300 1318 scans: background 150 1081 1081 1081 1081 1081 diamond 1214 1214 1214 f 2862 o of (FTIR) SWGDRUG.org/monographs.htm gain: 2914 1135 1135 1135 1135 1135 with 1401 2979 1400 3000 (Diamond 3057 1318 1318 1318 2862 2862 2862 1214 1214 1214 1214 1214 Resolution: Aperture: FTIR Number Sample Number 2862 2862 2862 1488 2914 2914 2914 1500 ATR 1401 1401 1401 2979 2979 2979 1401 1401 1401 2017 Enforcement Administration's Special 3057 3057 3057 1318 1318 1318 1318 1318 FTIR 2862 2862 2862 2862 2862 1488 1488 1488 14881618 1488 1488 1600 3500 2914 2914 2914 2914 2914 8/25/ generated this monograph using structurally Drug 1401 1401 1401 1401 1401 2979 2979 2979 2979 2979 1401 14011666 1401 1401 1401 3057 3057 3057 3057 3057 The 1700 14881618 1488 1618 1488 1618 1488 1488 1666 1666 1666 %Transmittance %Transmittance INFRARED SPECTROSCOPY 32 48 40 56 72 64 32 40 56 48 64 72 1618 1618 1618 1618 1618 Latest Revision: Latest Insrument: Scan Parameters: 3.3 1666 1666 1666 1666 1666 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.
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