Non-cyclol (lactame) ergot alkaloids

1982 ◽  
Vol 47 (12) ◽  
pp. 3312-3317 ◽  
Author(s):  
Josef Stuchlík ◽  
Alois Krajíček ◽  
Ladislav Cvak ◽  
Jiří Spáčil ◽  
Petr Sedmera ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Ergot Alkaloids ◽  
C Nmr

Two new alkaloids were isolated from the field ergot. Their structures, N-(D-lysergyl-L-valyl)cyclo(L-valyl-D-prolyl) (IV) and N-(D-lysergyl-L-valyl)cyclo(L-leucyl-D-prolyl) (V), were assigned by mass, 1H and 13C NMR spectroscopy.

The mechanism of formation of 2,7-dimethyl-2,6-octadiene in the synthesis of 3-methylene-7-methyl-1,6-octadiene

1983 ◽  
Vol 48 (7) ◽  
pp. 1864-1866
Author(s):  
Jan Bartoň ◽  
Ivan Kmínek
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Alkali Metal ◽  
Chromatographic Analysis ◽  
Solid Phase ◽  
Reaction Pathway ◽  
Mechanism Of Formation ◽  
Gas Chromatographic Analysis ◽  
C Nmr ◽  
Visual Observations

2,7-Dimethyl-2,6-octadiene is formed in the catalytic solution for the dimerization of 2-methyl-1,3-butadiene to β-myrcene (3-methylene-7-methyl-1,6-octadiene), as revealed by mass spectrometry and 13C NMR spectroscopy. Visual observations together with the results of gas chromatographic analysis of the catalytic solution suggest that the formation of 2,7-dimethyl-2,6-octadiene is associated with the transition of the alkali metal (sodium) from the solid phase into the solution. A reaction pathway is suggested accounting for the formation of 2,7-dimethyl-2,6-octadiene in the system.

An unusual reaction of a bridged triterpenoid α-diketone with acetic anhydride

1991 ◽  
Vol 56 (12) ◽  
pp. 2917-2935 ◽  
Author(s):  
Eva Klinotová ◽  
Václav Křeček ◽  
Jiří Klinot ◽  
Miloš Buděšínský ◽  
Jaroslav Podlaha ◽  
...  
Keyword(s):  
Acetic Acid ◽  
Nmr Spectroscopy ◽  
Acetic Anhydride ◽  
Spectral Methods ◽  
X Ray Diffraction ◽  
X Ray ◽  
Mild Conditions ◽  
Condensation Products ◽  
Unsaturated Lactones ◽  
C Nmr

3β-Acetoxy-21,22-dioxo-18α,19βH-ursan-28,20β-olide (IIIa) reacts with acetic anhydride in pyridine under very mild conditions affording β-lactone IVa and γ-lactones Va and VIIa as condensation products. On reaction with pyridine, lactones Va and VIIa undergo elimination of acetic acid to give unsaturated lactones VIIIa and IXa, respectively. Similarly, the condensation of 20β,28-epoxy-21,22-dioxo-18α,19βH-ursan-3β-yl acetate (IIIb) with acetic anhydride leads to β-lactone IVb and γ-lactone Vb; the latter on heating with pyridine affords unsaturated lactone VIIIb and 21-methylene-22-ketone Xb. The structure of the obtained compounds was derived using spectral methods, particularly 1H and 13C NMR spectroscopy; structure of lactone IVa was confirmed by X-ray diffraction.

A New Dimeric Derivative of Ethoxyquin from Its Reaction with Alkylperoxy Radicals

1993 ◽  
Vol 58 (8) ◽  
pp. 1914-1918 ◽  
Author(s):  
Jaroslav Kříž ◽  
Luděk Taimr
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Peroxy Radicals ◽  
Methyl Group ◽  
Alkylperoxy Radicals ◽  
C Nmr

The structure of a new compound formed in the reaction of ethoxyquin with alkylperoxy radicals was resolved by 1H and 13C NMR spectroscopy (including COSY, NOESY, HHC RCT and SSLR INEPT techniques) and confirmed by mass spectrometry. The structure suggest participation of 4-methyl group of ethoxyquin in the deactivation of peroxy radicals. A mechanism of this reaction is proposed.

Reactivity of Sodium Hexaethyl-2,4-dicarba-nido-hexaborate(1-)

1999 ◽  
Vol 64 (6) ◽  
pp. 977-985 ◽  
Author(s):  
Bernd Wrackmeyer ◽  
Hans-Jörg Schanz ◽  
Wolfgang Milius ◽  
Catherine McCammon
Keyword(s):  
Mössbauer Spectroscopy ◽  
Nmr Spectroscopy ◽  
Structural Analysis ◽  
Hydrogen Atom ◽  
Mossbauer Spectroscopy ◽  
Sandwich Complex ◽  
X Ray ◽  
Bromo Derivative ◽  
Boron Tribromide ◽  
C Nmr

Sodium hexaethyl-2,4-dicarba-nido-hexaborate(1-) (6), available from hexaethyl-2,4-dicarba- nido-hexaborane(8) (4) by deprotonation, reacts with deuterated methanol, CD3OD, to give back 4 without H/D exchange of the B-H-B hydrogen atom. The reaction of 6 with diethylboron chloride, Et2BCl, affords hexaethyl-2,4-dicarba-closo-hexaborane(6) (7), the first example of a peralkylated carborane of this type. In contrast, the reaction of 6 with boron tribromide, BBr3, leads mainly to 2,3,4,5,6,7-hexaethyl-2,4-dicarba-closo-heptaborane(7) (8), together with the corresponding 1-bromo derivative (9) and the closo-carborane 7 as side products. The reaction of two equivalents of 6 with FeCl2 gives the air-stable sandwich complex bis[hexaethyl-2,4-dicarba-nido-hexaborate(1-)]iron 10 which was characterised by X-ray structural analysis. All products were characterised by 1H, 11B and 13C NMR spectroscopy, and 57Fe Mössbauer spectroscopy was used to study 10.

Formation of spiro adduct from N-methyl-N-(2,4,6-trinitrophenyl)glycine anion

1989 ◽  
Vol 54 (2) ◽  
pp. 440-445 ◽  
Author(s):  
Vladimír Macháček ◽  
Alexandr Čegan ◽  
Miloš Sedlák ◽  
Vojeslav Štěrba
Keyword(s):  
Nmr Spectroscopy ◽  
Dimethyl Sulfoxide ◽  
Equilibrium Constant ◽  
Mole Fraction ◽  
Nucleophilic Addition ◽  
Adduct Formation ◽  
First Case ◽  
C Nmr

The intramolecular nucleophilic addition of N-methyl-N-(2,4,6-trinitrophenyl)glycine anion in methanol-dimethyl sulfoxide mixtures produces spiro[(3-methyl-5-oxazolidinone)-2,1'-(2',4',6'-trinitrobenzenide)]. The spiro adduct has been identified by means of 1H and 13C NMR spectroscopy. This is the first case when the formation of a Meisenheimer adduct with carboxylate ion is observed. Logarithm of the equilibrium constant of adduct formation increases linearly with the mole fraction of dimethyl sulfoxide in its mixture with methanol.

Alterations in Molecular Composition of Humic Substances from Eucalypt Plantation Soils Assessed by 13 C-NMR Spectroscopy

2012 ◽  
Vol 77 (1) ◽  
pp. 293-306 ◽  
Author(s):  
Emanuelle Mercês Barros Soares ◽  
Ivo Ribeiro Silva ◽  
Roberto Ferreira de Novais ◽  
Yan-Yan Hu ◽  
Klaus Schmidt-Rohr
Keyword(s):  
Nmr Spectroscopy ◽  
Humic Substances ◽  
Molecular Composition ◽  
Eucalypt Plantation ◽  
C Nmr

The Chlorination of Di-tert-butyl-2-naphthol+

1984 ◽  
Vol 39 (10) ◽  
pp. 1427-1432
Author(s):  
Edgar Streich ◽  
Anton Rieker
Keyword(s):  
Nmr Spectroscopy ◽  
Tert Butyl ◽  
Chlorine Substitution ◽  
C Nmr

Chlorination of the di-tert-butylation product of 2-naphthol leads to 3,6-di-tert-butyl-1,1-dichloro- l,2-dihydronaphthalen-2-one (4a) instead of 1,6-di-tert-butyl-1,3-dichloro-1,2-dihydronaphthalen-2-one (2) as reported [2], The structural proof was mainly offered by 13C NMR spectroscopy. The influence of annelation and chlorine substitution in 1,2-dihydronaphthalen-2-ones on δ13c=o is discussed, which is of importance for the use of δ13c=o for a general discrimination between ortho- and para-quinolide structures.

A Novel Method for 13C-NMR Spectroscopy of Polymer in Emulsion: Quantitative Analysis of Microstructure of Crosslinked Polybutadiene in Latex

1999 ◽  
Vol 72 (5) ◽  
pp. 844-853 ◽  
Author(s):  
Seiichi Kawahara ◽  
Saori Bushimata ◽  
Takashi Sugiyama ◽  
Chihiro Hashimoto ◽  
Yasuyuki Tanaka
Keyword(s):  
Nmr Spectroscopy ◽  
High Resolution ◽  
13C Nmr ◽  
Lattice Relaxation ◽  
13C Nmr Spectroscopy ◽  
Lattice Relaxation Time ◽  
Solid Sample ◽  
Spin Lattice Relaxation ◽  
High Resolution Spectrum ◽  
C Nmr

Abstract A novel analytical method using high resolution 13C-NMR spectroscopy to study polymer latex, which is a heterogeneous system comprising polymer dispersoid and water, is described. The appropriate concentrations of surfactant and dried rubber content of a polybutadiene latex, which give the best spectrum, were found to be 1 w/v % and 10%, respectively. The half-widths of resonance peaks for the latex sample were almost identical to the half-widths obtained in solution, which were about one-third the width of those obtained using a solid sample of either a crosslinked or soluble polybutadiene. Nevertheless, the signal to noise ratio for the latex sample was slightly smaller than that for the solution sample. The values of spin-lattice relaxation time, T1, for the latex sample were similar to those for the solid sample. These demonstrate that the latex state C-NMR spectroscopy will be a powerful technique for structural characterization of crosslinked gels in the dispersoid because it gives a high resolution spectrum comparable to solution state spectroscopy, showing short T1 values corresponding to those for solid state C-NMR spectroscopy. High resolution latex state 13C-NMR spectroscopy was used to determine the concentrations of the various isomers of the polybutadiene in the dispersoid.

Synthesis, Characterization and Complexation Studies with K + and Ca2+ Cations of trans-1.2-Cyclohexanedioxydiacetamides

1988 ◽  
Vol 43 (2) ◽  
pp. 165-170 ◽  
Author(s):  
Whei Oh Lin ◽  
Maria C. B. V. de Souza ◽  
Helmut G. Alt
Keyword(s):  
Nmr Spectroscopy ◽  
Mass Spectroscopy ◽  
H Nmr ◽  
Coordination Sites ◽  
Complexation Studies ◽  
Ir And Nmr Spectroscopy ◽  
Elemental Analyses ◽  
C Nmr

The synthesis of trans-1.2-cyclohexanedioxydiacetamides starting with trans-1.2-cyclohexane-diol is described. Eleven of these compounds are characterized by IR, 1H NMR, 13C NMR and mass spectroscopy as well as elemental analyses. Most of these compounds are suitable ionophors for the cations K+ and Ca2+. The coordination sites of these ligands in the 1:2 complexes were determined by IR and NMR spectroscopy

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