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
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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
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