The chlorination of some N,N-Dimethylanilines with 1,3,5-Trichloro-1,3,5-triazine-2,4,6(1H,3H,5H)-trione (Trichloroisocyanuric acid)

1980 ◽  
Vol 33 (4) ◽  
pp. 843 ◽  
Author(s):  
J Rosevear ◽  
JFK Wilshire

The reaction of some representative N,N-dimethylanilines and of Fischer's base (1,3,3-trimethyl-2-methyleneindoline) with trichloroisocyanuric acid in concentrated sulfuric acid has been investigated. In many cases mixtures of chlorinated products were obtained; these mixtures were examined both by gas-liquid chromatography and by proton magnetic resonance spectroscopy. The reaction of N,N-dimethylaniline with dichloroisocyanuric acid was also studied. ��� A feature of these chlorinations is the marked tendency for substitution to occur ortho to the dimethylamino group. This behaviour therefore differs from that reported for the corresponding brominations involving dibromoisocyanuric acid, where meta-substitution was observed.

1977 ◽  
Vol 30 (7) ◽  
pp. 1561 ◽  
Author(s):  
J Rosevear ◽  
JFK Wilshire

The reaction of some representative N,N-dimethylanilines with dibromoisocyanuric acid has been investigated. In many cases, mixtures of brominated products were obtained; these mixtures were analysed both by gas-liquid chromatography and by proton magnetic resonance spectroscopy. With excess of reagent, perbromination was readily achieved. ��� Significant solvent shifts [δ(CDCl3)-δ(C6D6)] were observed for a wide variety of bromo-N,N-dimethylanilines. This solvent shift phenomenon was used not only for the assignment of structure to reaction products but also for the quantitative analysis of mixtures of bromo-N,N-dimethylanilines.


1975 ◽  
Vol 151 (3) ◽  
pp. 491-495 ◽  
Author(s):  
J P Kamerling ◽  
G J Gerwig ◽  
J F G Vliegenthart ◽  
J R Clamp

The quantitative analysis by gas chromatography of monosaccharides present in glycoproteins and glycopeptides using methanolysis, followed by re-N-acetylation and trimethylsilylation, gives rise to several peaks for each monosaccharide. The identity of these peaks for xylose, fucose, mannose, galactose, glucose, N-acetylglucosamine, N-acetylgalactosamine and N-acetylneuraminic acid was established for α- and β-methyl pyranosides and furanosides by combined g.l.c.-mass spectrometry and proton-magnetic-resonance spectroscopy. These data provide for the unambiguous interpretation of the gas chromatograms obtained in the application of this g.l.c. method, and supply basic information for the further application of mass spectrometry in this field.


Intelligence ◽  
2009 ◽  
Vol 37 (2) ◽  
pp. 192-198 ◽  
Author(s):  
Rex E. Jung ◽  
Charles Gasparovic ◽  
Robert S. Chavez ◽  
Arvind Caprihan ◽  
Ranee Barrow ◽  
...  

1973 ◽  
Vol 56 (1) ◽  
pp. 124-127 ◽  
Author(s):  
Eric B Sheinin ◽  
Walter R Benson ◽  
Myron M Smith

Abstract Disulfiram was determined in disulfiram drug substance and tablets by proton magnetic resonance (PMR) spectroscopy at the 100–480 mg level and by a colorimetric technique involving cuprous iodide at the 50 mg level. The tablet excipients do not interfere in the analysis. The average result for disulfiram in a tablet composite was 100.8±1.4% of label claim by PMR and 100.7±0.4% by the colorimetric method.


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