Cycloaddition reactions of SNSAsF6 with aryl nitriles and diphenylacetylene; the preparation and characterization of aryl 1,3,2,4- and 1,2,3,5-dithiadiazole radicals

1992 ◽  
Vol 70 (12) ◽  
pp. 2972-2979 ◽  
Author(s):  
Jack Passmore ◽  
Xiaoping Sun ◽  
Simon Parsons
Keyword(s):  
Mass Spectrometry ◽  
Ionization Potentials ◽  
Cycloaddition Reactions ◽  
Neutral Radical ◽  
Aryl Nitriles ◽  
Elemental Analyses ◽  
Pure Compounds ◽  
Ft Raman

The SNS+ cation (in SNSAsF6) underwent symmetry-allowed concerted cycloadditions with the aryl nitriles RCN (R = 2,5-Me2C6H3, Ph, p-O2NC6H4, and 3,5-(O2N)2C6H3) and diphenylacetylene. The cycloadducts [Formula: see text] (R = 2,5-Me2C6H3, Ph, p-O2NC6H4, and 3,5-(O2N)2C6H3) and Ph [Formula: see text] were characterized by elemental analyses and IR and NMR (1H, 13C, 14N) spectroscopies. The reduction of [Formula: see text] gave the corresponding 1,3,2,4-dithiadiazoles [Formula: see text], which in turn rearranged to the corresponding 1,2,3,5-dithiadiazoles [Formula: see text]. The rate of this rearrangement was correlated with the ionization potentials of the corresponding nitriles. The radicals [Formula: see text] (R = Ph, p-O2NC6H4) were isolated as pure compounds, and characterized by mass spectrometry, IR, FT-Raman, and ESR spectroscopies. The reduction of [Formula: see text] led to neutral radical [Formula: see text], which is stable in solution up to ca. 0.5 M, but decomposes at higher concentrations.

Syntheses and Characterization of 1-Haloazagermatranes

2001 ◽  
Vol 56 (2) ◽  
pp. 137-140 ◽  
Author(s):  
Pavel L. Shutov ◽  
Sergey S. Karlov ◽  
Jörg Lorberth ◽  
Galina S. Zaitseva
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Molecular Composition ◽  
High Yield ◽  
Elemental Analyses ◽  
New Compounds ◽  
C Nmr

Abstract Germanium, Azagermatranes The reaction of tris(dimethylamino)halogermanes, (Me2N)3GeHal (7, Hal = Cl; 8 , Hal = Br), with tris(2-aminoethyl)amines, N(CH2CH2NHR)3 (5, R = H; 6 , R = Me), yield l-halo-N,N',N"-azagermatranes (1, X = Cl, R = H; 2, X = Br, R = H; 3, X = Cl, R = Me; 4, X = Br, R = Me). Treatment of 4 with n-butyllithium affords l-n-butyl-N,N',N"-trimethylazagermatrane (14) in high yield. Reactions of n-BuLi with 7 or (Me2N)4Ge (13) lead to the formation of (Me2N)3Ge-n-Bu (15). On treatment of 15 with 5 the 1 -n-butylazagermatrane 16 was obtained. The molecular composition and the structures of all new compounds were established by elemental analyses, 1H and 13C NMR spectroscopy and mass spectrometry.

Synthesis and Characterization of 1-Allyl-3,7,10-trimethylgermatrane and 1-Allylazagermatranes

1998 ◽  
Vol 53 (11) ◽  
pp. 1255-1258 ◽  
Author(s):  
Galina S. Zaitseva ◽  
Bettina A. Siggelkow ◽  
Sergey S. Karlov ◽  
Gleb V. Pen’kovoy ◽  
Jörg Lorberth
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Synthesis And Characterization ◽  
Elemental Analyses ◽  
New Compounds ◽  
C Nmr

The reaction between Br3GeAll (1) and N(CH2CHMeOSnBu3)3 (2, mixture of isomers) yielded N(CH2CHMeO)3GeAll (3) as a mixture of diastereomers. Three azagermatranes of the type N(CH2CH2NR)3GeAll (9, R = H; 10, R = Me; 11, R = Me3Si) have been synthesized from the reaction of (Me2N)3GeAll (5) with N (CH2CH2NHR)3 (R = H, 6; Me, 7; Me3Si, 8). Composition and structures of the new compounds were established by elemental analyses, 1H and 13C NMR spectroscopy and mass spectrometry.

Free Radicals by Mass Spectrometry. XLIII. Ionization Potentials and Ionic Heats of Formation for Vinyl, Allyl, and Benzyl Radicals

1971 ◽  
Vol 49 (3) ◽  
pp. 357-362 ◽  
Author(s):  
F. P. Lossing
Keyword(s):  
Mass Spectrometry ◽  
Electron Beam ◽  
Free Radicals ◽  
Ionization Potentials ◽  
Dissociative Ionization ◽  
Heats Of Formation ◽  
Neutral Radical ◽  
Benzyl Radical ◽  
Benzyl Cation ◽  
Benzyl Radicals

Using an energy-resolved electron beam, ionization potentials for the following free radicals have been measured: vinyl 8.95 V, allyl 8.07 V, benzyl 7.27 V. For vinyl and allyl ions new measurements of thresholds for dissociative ionization give ΔHf(C2H3+) = 266 kcal/mol and ΔHf(C3H5+) = 226 kcal/mol, leading to neutral radical heats of formation ΔHf(C2H3) = 59.6 kcal/mol and ΔHf(C3H5) = 40 kcal/mol. The data for benzyl radical and ion give ΔHf(benzyl cation) = 213 kcal/mol.

scholarly journals Synthesis, characterization and DNA interaction studies of new triptycene derivatives

2014 ◽  
Vol 10 ◽  
pp. 1290-1298 ◽  
Author(s):  
Sourav Chakraborty ◽  
Snehasish Mondal ◽  
Rina Kumari ◽  
Sourav Bhowmick ◽  
Prolay Das ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Conformational Changes ◽  
Dna Interaction ◽  
High Yield ◽  
Efficient Synthesis ◽  
Elemental Analyses ◽  
Multinuclear Nmr Spectroscopy ◽  
Propiolic Acid

A facile and efficient synthesis of a new series of triptycene-based tripods is being reported. Using 2,6,14- or 2,7,14-triaminotriptycenes as synthons, the corresponding triazidotriptycenes were prepared in high yield. Additionally, we report the transformation of 2,6,14- or 2,7,14-triaminotriptycenes to the corresponding ethynyl-substituted triptycenes via their tribromo derivatives. Subsequently, derivatization of ethynyl-substituted triptycenes was studied to yield the respective propiolic acid and ethynylphosphine derivatives. Characterization of the newly functionalized triptycene derivatives and their regioisomers were carried out using FTIR and multinuclear NMR spectroscopy, mass spectrometry, and elemental analyses techniques. The study of the interaction of these trisubstituted triptycenes with various forms of DNA revealed interesting dependency on the functional groups of the triptycene core to initiate damage or conformational changes in DNA.

Synthesis and Characterization of Chromium Tricarbonyl Complexes of 1-Phenylgermatrane and 1-Phenylazagermatrane. Crystal Structure of [N(CH2CH2O)3GeC6H5]Cr(CO)3

2002 ◽  
Vol 57 (9) ◽  
pp. 993-998 ◽  
Author(s):  
Sergey S. Karlov ◽  
Denis A. Sorokin ◽  
Yuri F. Oprunenko ◽  
Jörg Lorberth ◽  
Galina S. Zaitseva
Keyword(s):  
Crystal Structure ◽  
Mass Spectrometry ◽  
Nmr Spectroscopy ◽  
Synthesis And Characterization ◽  
Chromium Tricarbonyl ◽  
Elemental Analyses ◽  
Chromium Tricarbonyl Complexes ◽  
C Nmr

The reaction of 1-phenylgermatrane (1) and 1-phenylazagermatrane (2) with Cr(CO)6 affords chromium tricarbonyl complexes [N(CH2CH2O)3GeC6H5]Cr(CO)3 (6) and [N(CH2- CH2NH)3GeC6H5]Cr(CO)3 (7). In contrast, the same reaction of Cr(CO)6 with 1-(9-anthracenyl) germatrane (3) does not proceed. Composition and structures of the 6 and 7 were established by elemental analyses, 1H and 13C NMR spectroscopy and mass spectrometry. The crystal structure of 6 is reported

Deep proteomic characterization of fiber types of murine muscles by laser microdissection and mass spectrometry

2019 ◽  
Author(s):  
B Eggers ◽  
K Schork ◽  
R Schröder ◽  
CS Clemen ◽  
C Berwanger ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Laser Microdissection ◽  
Fiber Types
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