PROTON MAGNETIC RESONANCE AND INFRARED SPECTRA OF SOME COMPLEXES OF N,N-DIMETHYLACETAMIDE

1966 ◽  
Vol 44 (16) ◽  
pp. 1881-1887 ◽  
Author(s):  
A. J. Carty
Keyword(s):  
Magnetic Resonance ◽  
Complex Formation ◽  
Infrared Spectra ◽  
Proton Magnetic Resonance ◽  
Low Field ◽  
New Compounds ◽  
Solid Complexes ◽  
Magnetic Resonance Spectra

Proton magnetic resonance spectra of some complexes of In, Zn, Cd, and Sn halides and perchlorates with N,N-dimethylacetamide (DMA) have been measured in acetone-d6. Low field shifts of the methyl resonances of DMA on complex formation are dependent on metal and anion. The similarity of the spectra of all the complexes suggests only oxygen-coordinated DMA in solution. Infrared spectra in the range 2 000–625 cm−1 are recorded. Changes in the C—O and C—N stretching frequencies of the ligand on coordination are consistent with oxygen-bonded DMA both in the solid complexes and in solution.The new compounds Zn(ClO4)2•6DMA, Cd(ClO4)2•6DMA, CdI2•2DMA, and SnCl4•2DMA are reported.

Investigation and Identification of the Bromination Products of Dimethoxyamphetamines

1976 ◽  
Vol 59 (5) ◽  
pp. 1162-1169
Author(s):  
Keith Bailey ◽  
Denise R Gagné ◽  
Richard K Pike
Keyword(s):  
Magnetic Resonance ◽  
Qualitative Analysis ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Infrared Spectra ◽  
Proton Magnetic Resonance ◽  
Positive Identification ◽  
Aromatic Bromination ◽  
Layer Chromatography ◽  
Magnetic Resonance Spectra

Abstract The qualitative analysis of the aromatic bromination products of the 6 isomeric dimethoxyamphetamines and their hydrochloride or hydrobromide salts is described. Their ultraviolet, mass, and proton magnetic resonance spectra are not sufficiently different for distinction but infrared spectra allow a positive identification to be made and reference spectra are provided for the bromination products of 2,4-, 2,5-, 2,6-, 4,5-, and 3,5-dimethoxyamphetamines. The application of gas-liquid and thin layer chromatography for the analysis of these products is discussed. The bromination of 2,3-dimethoxyamphetamine consistently gave mixtures which could not be separated satisfactorily; spectra are included for completeness of the comparison of products.

Spectroscopic Properties of the Methyl Esters of Chlorophenoxy Acid Herbicides

1975 ◽  
Vol 58 (5) ◽  
pp. 1001-1012 ◽  
Author(s):  
Carlos H Van Peteghem ◽  
Aubin M Heyndrickx
Keyword(s):  
Magnetic Resonance ◽  
Infrared Spectra ◽  
Proton Magnetic Resonance ◽  
Mass Spectra ◽  
Methyl Esters ◽  
Spectroscopic Properties ◽  
Chlorophenoxy Acid Herbicides ◽  
Acid Herbicides ◽  
Magnetic Resonance Spectra

Abstract The mass and infrared spectra of the methyl esters of 9 chlorophenoxy acid herbicides are presented. Ultraviolet data are discussed and proton magnetic resonance spectra are tabulated. Because of the sensitivity of the technique, the mass spectra are most useful for the identification of those compounds in residues, especially by combined gas chromatographymass spectrometry. The pure herbicides used for the recording of the spectra were obtained by synthesis and recrystallization.

Distinction of Some Dialkyl Amides of Lysergic and iso-Lysergic Acids from LSD

1973 ◽  
Vol 56 (1) ◽  
pp. 88-99
Author(s):  
Keith Bailey ◽  
Denise Verner ◽  
Donald Legault
Keyword(s):  
Magnetic Resonance ◽  
Thin Layer ◽  
Infrared Spectra ◽  
Proton Magnetic Resonance ◽  
Mass Spectra ◽  
Structural Identification ◽  
Lysergic Acid ◽  
Ultraviolet Spectra ◽  
Liquid Chromatographic ◽  
Magnetic Resonance Spectra

Abstract The 10 lysergic and iso-lysergic acid amides described are N,N-dimethyl-, N,N-diethyl-, N-methyl-N-propyl, N-ethyl-N-propyl, and N,N-dipropyl-. Their ultraviolet spectra are insufficiently different for distinction. Mass spectra do not readily differentiate between isomers. Proton magnetic resonance spectra are distinct and provide a positive structural identification of the amide. Their infrared spectra are similar, but suitable for distinguishing these compounds from LSD. Various reference spectra are provided. Thin layer and gas-liquid chromatographic systems suitable for distinguishing these compounds from LSD are described.

Lanthanide Induced Shifts in the Proton Magnetic Resonance Spectra of Cyclic Amines

1973 ◽  
Vol 51 (24) ◽  
pp. 4080-4081 ◽  
Author(s):  
Donald L. Hooper ◽  
Alzbeta Kardos
Keyword(s):  
Magnetic Resonance ◽  
Complex Formation ◽  
Proton Magnetic Resonance ◽  
Steric Effect ◽  
Cyclic Amines ◽  
Lanthanide Induced Shifts ◽  
Magnetic Resonance Spectra

Complex formation between europium tris(dipivalatomethane), Eu(DPM)3, and cyclic amines is not accompanied by inversion of the amine configuration, even for 2-alkyl and 2,6-dialkylpiperidines, where inversion of the amine configuration accompanies formation of the usual amine derivatives. There is, however, a steric effect of C-2 or C-6 substitution, in that the magnitude of the lanthanide induced shifts is sharply reduced.

Proton magnetic resonance spectra of vinylmetallic compounds. Part I. Tetravinyl and triphenylvinyl derivatives of Group IVB elements

1968 ◽  
Vol 46 (14) ◽  
pp. 2373-2384 ◽  
Author(s):  
Seán Cawley ◽  
Steven S. Danyluk
Keyword(s):  
Magnetic Resonance ◽  
Proton Magnetic Resonance ◽  
Phenyl Group ◽  
Coupling Constants ◽  
Multiple Quantum ◽  
Low Field ◽  
Diamagnetic Anisotropy ◽  
Vinyl Group ◽  
Derivatives Of ◽  
Magnetic Resonance Spectra

A study has been made of the proton magnetic resonance spectra for all of the Group IVB derivatives of the series MVi4 and [Formula: see text]([Formula: see text] = phenyl group and Vi = vinyl group). The spectra were measured at 60 MHz as accurately as possible and the assignment of transitions was checked with a variety of supplemental aids including double irradiation, multiple quantum transitions, and medium effects Final, accurate spectral parameters were derived using both iterative and exact computational methods for solution of the three-spin problem Excellent agreement was obtained between the sets of parameters determined by the two methodsThe chemical shifts for both series of compounds display a number of characteristic trends of which the most notable is a displacement of the vinyl proton signals to low field with increasing atomic number of the M atom In each series the largest shift change is noted in going from the carbon to the silicon derivative These deshieldings have been attributed to the enhanced possibility of dπ–pπ interaction between the central M atom and the vinyl group in higher members of the series Marked changes are also the internal shifts of the vinyl protons down both series of compounds It is concluded that these changes are principally due to the effects of the M—C bond diamagnetic anisotropy The trends in internal shifts can be satisfactorily reproduced by the dipole approximation using Δχ values of 4, 6, 8, 12, and 18 × 10−6 cm3 mole−1 for the C, Si, Ge, Sn, and Pb–carbon bonds respectivelyThe signals for the vinyl protons of the [Formula: see text] series are all located to low field relative to the MVi4 series This deshielding is satisfactorily accounted for by the effects of the phenyl ring diamagnetic anisotropy in the former seriesA linear correlation is observed between the sums of the coupling constants and the electronegativities, Em, of the central M atom for both series of compounds However, the ΣJ values for the [Formula: see text] series are all slightly lower than the corresponding sums for the MVi4 series, indicating that the electronegativity of the phenyl group is somewhat larger than for the vinyl groupA significant solvent and concentration dependence is only noted for compounds belonging to the [Formula: see text] series For example, the trans proton of [Formula: see text] shifts up-field by 4 Hz while the cis proton is displaced down-field by 4 Hz as the concentration of [Formula: see text] is increased to 50 mole % in carbon tetrachloride These changes have been interpreted on the basis of a solute–solute interaction scheme of the type proposed previously for phenyl proton shifts.

Identification of Some Analogs of the Hallucinogen Phencyclidine

1976 ◽  
Vol 59 (1) ◽  
pp. 81-89 ◽  
Author(s):  
Keith Bailey ◽  
Denise R Gagné ◽  
Richard K Pike
Keyword(s):  
Magnetic Resonance ◽  
Thin Layer ◽  
Infrared Spectra ◽  
Proton Magnetic Resonance ◽  
Spectroscopic Techniques ◽  
Magnetic Resonance Spectra

Abstract The drugs 1-[1-(2-thienyl)cyclohexyl]piperidine, 1-[1-(2-thienyl) cyclohexyl] morpholine, 1-[1-(2-thienyl)cyclohexyl] pyrrolidine, 1-(1-phenylcyclohexyl) morpholine, and 1-(1-phenylcyclohexyl) pyrrolidine are identified by spectroscopic techniques. The ultraviolet and proton magnetic resonance spectra of analogs are similar, but mass and infrared spectra are distinctly different, and reference spectra are provided. Gas-liquid and thin layer chromatographic systems for the analysis are discussed.

The preparation of 2-Fluoro-5-nitrobenzonitrile and the proton magnetic resonance spectra of some compounds containing the N-(2-Cyano-4-nitrophenyl) group

1967 ◽  
Vol 20 (8) ◽  
pp. 1663 ◽  
Author(s):  
JFK Wilshire
Keyword(s):  
Amino Acids ◽  
Magnetic Resonance ◽  
Nitro Group ◽  
Proton Magnetic Resonance ◽  
Cyano Group ◽  
Aromatic Nucleus ◽  
Heteroaromatic Compounds ◽  
Magnetic Resonance Spectra

2-Fluoro-5-nitrobenzonitrile, an analogue of 1-fluoro-2,4- dinitrobenzene, in which the 2-nitro group has been replaced by a cyano group, has been prepared and made to react with several amines, amino acids, and NH-heteroaromatic compounds. The proton magnetic resonance spectra of some of the resultant N-(2-cyano-4-nitrophenyl) derivatives were compared with the spectra of the corresponding N-(2,4- dinitrophenyl) derivatives and furnish further evidence that the ortho nitro group of the latter derivatives is rotated out of the plane of the aromatic nucleus.

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