Gas chromatographic-mass spectral analyses of s-triazine metabolites

1978 ◽  
Vol 26 (3) ◽  
pp. 635-638 ◽  
Author(s):  
William R. Lusby ◽  
Philip C. Kearney
Keyword(s):  
Spectral Analyses ◽  
Mass Spectral ◽  
Chromatographic Mass

Solvolytic rearrangement studies with 14C or 13C labeled (E)- and (Z)-1,2-diphenyl-2-tolylvinyl bromides

1986 ◽  
Vol 64 (6) ◽  
pp. 1228-1234
Author(s):  
Choi Chuck Lee ◽  
Dave Wanigasekera
Keyword(s):  
Detectable Amount ◽  
Spectral Analyses ◽  
Mass Spectral ◽  
Vinyl Bromide ◽  
Product Mixture ◽  
Pure Product ◽  
Before And After ◽  
Chromatographic Mass

The reaction of (E)-, (Z)-, or a 2:3 mixture of (E)- and (Z)-1,2-diphenyl-2-tolyl[2-14C]vinyl bromide ((E)-, (Z)-, or (E,Z)-3-Br-2-14C) in HOAc–AgOAc gave a 1:1 mixture of the structurally unrearranged but isotopically scrambled (E)- and (Z)-1,2-diphenyl-2-tolyl[1,2-14C]vinyl acetates ((E,Z)-3-OAc-1,2-14C), with an average of 18.3% scrambling of the 14C label from C-2 to C-1 arising from 1,2-tolyl shifts in the 1,2-diphenyl-2-tolylvinyl cation (3). No detectable amount of the structurally rearranged 2,2-diphenyl-1-tolylvinyl acetate (4-OAc) was formed. Solvolysis of (E,Z)-3-Br-2-14C in TFE-2,6-lutidine gave as products 62% 4-OTFE-1,2-14C and 38% of a 1:1 mixture of (E)- and (Z)-3-OTFE-1,214C. Only (Z)-3-OTFE-1,2-14C could be isolated as a pure product and it showed an average of 44.7% scrambling of the label from C-2 to C-1. Similar trifluoroethanolyses of (E,Z)-3-Br-2-13C coupled with gas chromatographic - mass spectral analyses of the diphenyl and phenyl tolyl ketones from ozonolysis of the product mixture showed 44.6% scrambling in the (E,Z)-3-OTFE-1,2-13C, confirming the 14C results for the (Z) isomer. Nondegenerate rearrangements from 1,2-phenyl shifts before and after the degenerate 1,2-tolyl shifts to give 4-OTFE-1-13C and 4-OTFE-2-13C were also observed, demonstrating the occurrence of successive 1,2-aryl shifts in these triarylvinyl cations.

Synthesis of Novel Bis-pyrazoles via Electrophilic Cyclization

2019 ◽  
Vol 16 (6) ◽  
pp. 511-516
Author(s):  
Adnan Cetin
Keyword(s):  
13C Nmr ◽  
Cyclization Reaction ◽  
Electrophilic Cyclization ◽  
Pyrazole Derivatives ◽  
Spectral Analyses ◽  
Mass Spectral ◽  
Palladium Catalyzed ◽  
Ft Ir ◽  
Reaction Compound

Efficient steps towards the synthesis of novel (phenyl)(1'-aryl-1,5,5'-triphenyl[3,3'-bi-1Hpyrazol]- 4-yl)methanones 4a-e were developed. The procedure starts from 1-(4-benzoyl-1,5-diphenyl- 1H-3-pyrazolyl)-3-phenyl-2-propyn-1-one (2) which was synthesized by a palladium catalyzed crosscoupling reaction. Compound 2 reacted with various hydrazines to give (E)-(phenyl)[1,5-diphenyl-3- [3-phenyl-1-(2-arylhydrazono)-2-propyn-1-yl]-1H-4-pyrazolyl]methanones E-3a-e. The bis-pyrazole derivatives 4a-e were synthesized from electrophilic cyclization reaction of α,β-acetylenic hydrazones E-3a-e and copper(I) iodide. All synthesized compounds were characterized by FT-IR, 1H, 13C NMR and Mass spectral analyses.

Electron capture gas-liquid chromatographic-mass spectral identification of acids produced by Neisseria meningitidis in a defined medium

1979 ◽  
Vol 9 (1) ◽  
pp. 97-102
Author(s):  
C C Alley ◽  
J B Brooks ◽  
D S Kellogg
Keyword(s):  
Liquid Chromatography ◽  
Neisseria Meningitidis ◽  
Electron Capture ◽  
Defined Medium ◽  
Gas Liquid Chromatography ◽  
Mass Spectral ◽  
Spectral Identification ◽  
Acid Metabolites ◽  
Liquid Chromatographic ◽  
Chromatographic Mass

The acid metabolites and the cellular fatty acids of three strains of Neisseria meningitidis grown in a chemically defined liquid medium were determined with computerized frequency-pulsed electron capture gas-liquid chromatography. Five acids not previously reported were subsequently identified: isobutyric, octanoic, decenoic (C10:1), dodecenoic (C12:1), and tetradecenoic (C14:1). These acids were produced during active metabolism and were not detected as cellular constituents. The frequency-pulsed electron capture gas-liquid chromatography methods which we used provide a rapid, reliable, sensitive means of detecting both these and other metabolic and cellular acids in spent culture medium.

Combined Gas-Liquid Chromatographic Mass Spectrometric Analysis of Some Commercial Aryl Phosphate Oils

1978 ◽  
Vol 61 (2) ◽  
pp. 266-271
Author(s):  
Padmakar G Deo ◽  
Philip H Howard
Keyword(s):  
Fire Retardant ◽  
Phosphate Esters ◽  
Spectrometric Analysis ◽  
Gas Liquid Chromatography ◽  
Mass Spectral Data ◽  
Mass Spectral ◽  
Hydraulic Fluids ◽  
Alkyl Phenols ◽  
Liquid Chromatographic ◽  
Chromatographic Mass

Abstract Five commercial samples of synthetic aryl phosphate oils, which are widely used as fire retardant hydraulic fluids and as flame retardant plasticizers, have been analyzed by combined gas-liquid chromatography/mass spectrometry (GLC/MS). Each sample contained at least 4 isomers of aryl phosphate esters. The peaks were identified by a close examination of the mass spectral data and, wherever possible, by comparing retention times of the peaks with those of either the purchased or synthesized compounds. One aryl phosphate hydraulic fluid contained a small amount of a hydrocarbon. The results indicate that most of the aryl phosphate esters in the commercial samples were formed from phenol, cresols, xylenols, and other alkyl phenols. No free phenols could be detected in the samples analyzed.

Characterization of Drinking Water Odour Arising from Spring Thaw for an Ice-Covered Upland River Source

1992 ◽  
Vol 25 (2) ◽  
pp. 65-72 ◽  
Author(s):  
S. E. Hrudey ◽  
D. Rector ◽  
N. Motkosky
Keyword(s):  
Drinking Water ◽  
Activated Carbon ◽  
Water Samples ◽  
Raw Water ◽  
Mass Spectral ◽  
The North ◽  
Water Conditions ◽  
Biogenic Source ◽  
Chromatographic Mass

Recurring odour events during spring thaw in the North Saskatchewan River led to a program to characterize contributing odour agents. Raw and treated water samples were adsorbed on granular activated carbon which was then exhaustively solvent extracted. The solvent concentrates were subjected to a Chromatographie sniffing procedure combined with gas chromatographic-mass spectral analyses. Geosmin and 2-methylisoborneol were identified by sensory and analytical means as likely major contributors to the raw water odour. Benzaldehyde, camphor and dihydroactinidiolide were other relevant compounds identified. Given the near freezing water conditions at the time of the odour event, the biogenic source of the odour agents remains a subject for investigation.

scholarly journals Composition of the Essential Oil of Wild Growing Artemisia vulgaris from Erie, Pennsylvania

2012 ◽  
Vol 7 (5) ◽  
pp. 1934578X1200700 ◽  
Author(s):  
Jack D. Williams ◽  
Ayman M. Saleh ◽  
Dom N. Acharya
Keyword(s):  
United States ◽  
Essential Oil ◽  
The United States ◽  
Artemisia Vulgaris ◽  
Mass Spectral Analysis ◽  
Mass Spectral ◽  
Aerial Parts ◽  
Germacrene D ◽  
Leaf Oil ◽  
Chromatographic Mass

Essential Oil from wild growing Artemisia vulgaris L. originating in Erie, Pennsylvania was obtained by hydrodistillation of the aerial parts of the plant. Gas chromatographic-mass spectral analysis was used to identify the major volatiles present. Up to 22 components were detected in the essential oils. Germacrene D (25%), Caryophyllene (20%), α-Zingiberene (15%) and Borneol (11%) represent the major components of leaf oil, while the buds were rich in 1,8-Cineole (32%), Camphor (16%), Borneol (9%), and Caryophyllene (5%). trans-2-Hexenal was also detected in the aerial parts of the plant. α-Zingiberene and trans-2-Hexenal have not been previously reported for Artemisia vulgaris L. The major analytes are compared to those from Artemisia vulgaris L, originating outside of the United States.

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