Clonazolam The Drug Enforcement Administration's Special ...Clonazolam The Drug Enforcement...

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Clonazolam The Drug Enforcement Administration's Special Testing and Research Laboratory generated this monograph using structurally confirmed reference material. Latest Revision: 10/18/16 SWGDRUG.org/monographs.htm Page 1 of 5 N N N C H 3 N N O O Cl 1. GENERAL INFORMATION IUPAC Name: 6-(2-chlorophenyl)-1-methyl-8-nitro-4 H-[1,2,4]triazolo[4,3-a][1,4]benzodiazepine CAS#: 33887-02-4 Synonyms: Clonitrazolam Source: DEA Reference Material Collection Appearance: Yellow powder UV max (nm): Not Determined 2. CHEMICAL AND PHYSICAL DATA 2.1 CHEMICAL DATA Form Chemical Formula Molecular Weight Melting Point ( o C) Base C 17 H 12 ClN 5 O 2 353 Not Determined

Transcript of Clonazolam The Drug Enforcement Administration's Special ...Clonazolam The Drug Enforcement...

ClonazolamThe Drug Enforcement Administration's Special Testing and Research Laboratory

generated this monograph using structurally confirmed reference material.

Latest Revision: 10/18/16 SWGDRUG.org/monographs.htm Page 1 of 5

N N

N

CH3

N

NO

O

Cl

1. GENERAL INFORMATION

IUPAC Name: 6-(2-chlorophenyl)-1-methyl-8-nitro-4H-[1,2,4]triazolo[4,3-a][1,4]benzodiazepine

CAS#: 33887-02-4

Synonyms: Clonitrazolam

Source: DEA Reference Material Collection

Appearance: Yellow powder

UVmax(nm): Not Determined

2. CHEMICAL AND PHYSICAL DATA

2.1 CHEMICAL DATA

Form Chemical Formula Molecular Weight Melting Point (oC)

Base C17H12ClN5O2 353 Not Determined

ClonazolamThe Drug Enforcement Administration's Special Testing and Research Laboratory

generated this monograph using structurally confirmed reference material.

8.5

Latest Revision: 10/18/16 SWGDRUG.org/monographs.htm Page 2 of 5

3. QUALITATIVE DATA

3.1 NUCLEAR MAGNETIC RESONANCE

Sample Preparation: Dilute analyte to ~15 mg/mL in deuterated methanol containing TMS for 0 ppmreference and dimethylsulfone 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 seconds1H NMR: Clonazolam Lot RM-151119-01; CD3OD; 400MHz

8 7 6 5 4 3 2 1 0

31112121

TMS

dimethylsulfone

from CD3OD from CD3OD

8.0 7.5

12121

5.40 5.35

1

4.425 4.375

1

2.675

3

ClonazolamThe Drug Enforcement Administration's Special Testing and Research Laboratory

generated this monograph using structurally confirmed reference material.

Latest Revision: 10/18/16 SWGDRUG.org/monographs.htm Page 3 of 5

3.2 GAS CHROMATOGRAPHY/MASS SPECTROMETRY

Sample Preparation: Dilute analyte ~3 mg/mL in methanol.

Instrument: Agilent gas chromatograph operated in split mode with MS detectorColumn: DB-5 MS (or equivalent); 30m x 0.25 mm x 0.25 µmCarrier Gas: Helium at 1 mL/minTemperatures: Injector: 280oC

MSD transfer line: 280oCMS Source: 250oCMS Quad: 150oCOven program:

1) 100oC initial temperature for 1.0 min2) Ramp to 280oC at 12 oC/min3) Hold final temperature for 9.0 min

Injection Parameters: Split Ratio = 25:1, 1 µL injectedMS Parameters: Mass scan range: 30-550 amu

Threshold: 150Tune file: stune.uAcquisition mode: scan

Retention Time: 17.99 minEI Mass Spectrum: Clonazolam Lot RM-151119-01

m/z340320300280260240220200180160140120100806040

0

8

16

24

32

40

48

56

64

72

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96

5151515151515151515151515151515151515151515163636363636363636363636363636363636363636363

75757575757575757575757575757575757575757575

7676767676767676767676767676767676767676767689898989898989898989898989898989898989898989

101101101101101101101101101101101101101101101101101101101101101101

102102102102102102102102102102102102102102102102102102102102102102

111111111111111111111111111111111111111111111111111111111111111111137137137137137137137137137137137137137137137137137137137137137137

142142142142142142142142142142142142142142142142142142142142142142 149149149149149149149149149149149149149149149149149149149149149149150150150150150150150150150150150150150150150150150150150150150150

176176176176176176176176176176176176176176176176176176176176176176177177177177177177177177177177177177177177177177177177177177177177

202202202202202202202202202202202202202202202202202202202202202202

203203203203203203203203203203203203203203203203203203203203203203

204204204204204204204204204204204204204204204204204204204204204204

238238238238238238238238238238238238238238238238238238238238238238

249249249249249249249249249249249249249249249249249249249249249249

278278278278278278278278278278278278278278278278278278278278278278

324324324324324324324324324324324324324324324324324324324324324324

326326326326326326326326326326326326326326326326326326326326326326

353353353353353353353353353353353353353353353353353353353353353353

EI+

ClonazolamThe Drug Enforcement Administration's Special Testing and Research Laboratory

generated this monograph using structurally confirmed reference material.

1700 1600 1500 1400 1300 1200 1100 1000 900 800 700 Wavenumber (cm-1) Latest Revision: 10/18/16 SWGDRUG.org/monographs.htm Page 4 of 5

3.3 INFRARED SPECTROSCOPY (FTIR)

Insrument: 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): Clonazolam Lot RM-151119-01

Wavenumber (cm-1)3500 3000 2500 2000 1500

%Tr

ansm

ittan

ce

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1612161216121612161216121612161216121612161216121612161216121612161216121612161216121612

1531153115311531153115311531153115311531153115311531153115311531153115311531153115311531

1519151915191519151915191519151915191519151915191519151915191519151915191519151915191519

14861486148614861486148614861486148614861486148614861486148614861486148614861486148614861428142814281428142814281428142814281428142814281428142814281428142814281428142814281428

1350135013501350135013501350135013501350135013501350135013501350135013501350135013501350

1321132113211321132113211321132113211321132113211321132113211321132113211321132113211321

10991099109910991099109910991099109910991099109910991099109910991099109910991099109910991058105810581058105810581058105810581058105810581058105810581058105810581058105810581058 1038

103810381038103810381038103810381038103810381038103810381038103810381038103810381038

999999999999999999999999999999999999999999999999999999999999999999

970970970970970970970970970970970970970970970970970970970970970970

878878878878878878878878878878878878878878878878878878878878878878

837837837837837837837837837837837837837837837837837837837837837837

776776776776776776776776776776776776776776776776776776776776776776

742742742742742742742742742742742742742742742742742742742742742742

726726726726726726726726726726726726726726726726726726726726726726

669669669669669669669669669669669669669669669669669669669669669669542542542542542542542542542542542542542542542542542542542542542542520520520520520520520520520520520520520520520520520520520520520520

%Tr

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1612161216121612161216121612161216121612161216121612161216121612161216121612161216121612

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1531153115311531153115311531153115311531153115311531153115311531153115311531153115311531

1519151915191519151915191519151915191519151915191519151915191519151915191519151915191519

1486148614861486148614861486148614861486148614861486148614861486148614861486148614861486

1470147014701470147014701470147014701470147014701470147014701470147014701470147014701470

1428142814281428142814281428142814281428142814281428142814281428142814281428142814281428

1402140214021402140214021402140214021402140214021402140214021402140214021402140214021402

1374137413741374137413741374137413741374137413741374137413741374137413741374137413741374

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1321132113211321132113211321132113211321132113211321132113211321132113211321132113211321

1250125012501250125012501250125012501250125012501250125012501250125012501250125012501250

1201120112011201120112011201120112011201120112011201120112011201120112011201120112011201

10991099109910991099109910991099109910991099109910991099109910991099109910991099109910991058105810581058105810581058105810581058105810581058105810581058105810581058105810581058 1038

103810381038103810381038103810381038103810381038103810381038103810381038103810381038

999999999999999999999999999999999999999999999999999999999999999999

970970970970970970970970970970970970970970970970970970970970970970

914914914914914914914914914914914914914914914914914914914914914914878878878878878878878878878878878878878878878878878878878878878878

837837837837837837837837837837837837837837837837837837837837837837

808808808808808808808808808808808808808808808808808808808808808808

776776776776776776776776776776776776776776776776776776776776776776

742742742742742742742742742742742742742742742742742742742742742742

726726726726726726726726726726726726726726726726726726726726726726

703703703703703703703703703703703703703703703703703703703703703703

669669669669669669669669669669669669669669669669669669669669669669

638638638638638638638638638638638638638638638638638638638638638638

550550550550550550550550550550550550550550550550550550550550550550 542

542542542542542542542542542542542542542542542542542542542542542520520520520520520520520520520520520520520520520520520520520520520

ClonazolamThe Drug Enforcement Administration's Special Testing and Research Laboratory

generated this monograph using structurally confirmed reference material.

Latest Revision: 10/18/16 SWGDRUG.org/monographs.htm Page 5 of 5

http://forendex.southernforensic.org/index.php/detail/index/1323

http://en.wikipedia.org/wiki/Clonazolam

4. ADDITIONAL RESOURCES

Forendex

Wikipedia