URB '-carbamoylbiphenyl-3-yl cyclohexylcarbamate. DEA Reference Material Collection. Form Chemical Formula Molecular Weight Melting Point ( o C)

Transcription

1 O NH O NH O. GENERAL INFORMATION IUPAC Name: 3'-carbamoylbiphenyl-3-yl cyclohexylcarbamate CAS#: Synonyms: Source: Appearance: UV max (nm): KDS-03 DEA Reference Material Collection White powder Not Determined. CHEMICAL AND PHYSICAL DATA. CHEMICAL DATA Form Chemical Formula Molecular Weight Melting Point ( o C) Base C 0 H N O Not Determined Page of 6

2 3. QUALITATIVE DATA 3. NUCLEAR MAGNETIC RESONANCE Sample Preparation: Dilute analyte to ~5 mg/ml incd 3 OD containing TMS for 0 ppm reference and maleic acid as quantitative internal standard. Instrument: Parameters: 00 MHz NMR spectrometer Spectral width: at least containing -3 ppm through 3 ppm Pulse angle: 90 o Delay between pulses: 5 seconds H NMR: Lot # ALB-3-; CD 3 OD; 00MHz Maleic Acid from CD3OD from CD3OD TMS Page of 6

3 3. GAS CHROMATOGRAPHY/MASS SPECTROMETRY Sample Preparation: Dilute analyte to ~ mg/ml in chloroform with 5 drops methanol. Instrument: Agilent gas chromatograph operated in split mode with MS detector Column: DB- MS (or equivalent); 30m x 0.5 mm x 0.5 µm Carrier Gas: Helium at ml/min Temperatures: Injector: 80 o C MSD transfer line: 80 o C MS Source: 30 o C MS Quad: 50 o C Oven program: ) 00 o C initial temperature for.0 min ) Ramp to 300 o C at o C/min 3) Hold final temperature for 9.0 min Injection Parameters: Split Ratio = 0:, µl injected MS Parameters: Mass scan range: amu Threshold: 00 Tune file: stune.u Acquisition mode: scan Retention Time: MWt 3:.96 min; MWt 5:.860 min. EI Mass Spectrum: (MWt 3) Lot # ALB-3- Intensity [x 0 ] EI m/z Page 3 of 6

4 Intensity [x 0 5 ] EI Mass Spectrum: (MWt 5) Lot # ALB EI m/z.860 TIC: Lot # ALB Retention Time (min) GC/MS Analytical Observation: is thermally unstable; therefore, no Electron Impact mass spectrum of the complete molecule could be obtained. Instead, the mass spectrum shows the presence of two compounds,one with a molecular weight of 3 and a second with a molecular weight of 5. The combined masses equal the molecular weight of. The mass spectra of the two compounds are shown above along with the TIC. Page of 6

5 Wavenumber (cm-) Page 5 of INFRARED SPECTROSCOPY (FTIR) Insrument: FTIR with diamond ATR attachment (3 bounce) Scan Parameters: Number of scans: 3 Number of background scans: 3 Resolution: cm - Sample gain: 8 Aperture: 50 FTIR ATR (Diamond, 3 Bounce): Lot # ALB-3- Wavenumber (cm-) %Transmittance %Transmittance

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