Massenspektrometrische Fragmentierung von Trimethylsilylderivaten (TMS) des Thyrotropin-„Releasing“-Hormons (TRH) und dessen Teilstrukturen / Mass Spectroscopy of Trimethylsilyl Derivatives of Thyrotropin-releasing Hormone and its Constituents

1973 ◽  
Vol 28 (11-12) ◽  
pp. 820-823 ◽  
Author(s):  
W. A. König ◽  
S. Fuchs ◽  
K. Zech ◽  
W. Voelter

The mass spectral fragmentation patterns of trimethylsilyl derivatives of TRH and its constituents are discussed. The utility of these derivatives for the control of the synthesis of peptide hormones by mass spectrometry is obvious.

2013 ◽  
Vol 8 (6) ◽  
pp. 1934578X1300800
Author(s):  
Vladimir A. Khripach ◽  
Danuše Tarkowská ◽  
Vladimir N. Zhabinskii ◽  
Olga V. Gulyakevich ◽  
Yurii V. Ermolovich ◽  
...  

New analogues of brassinolide biosynthetic precursors with three deuterium atoms at non-exchangeable positions have been synthesized to be used as standards for quantification of natural brassinosteroids by liquid chromatography-mass spectrometry. [26-2H3](22 R,23 R,24 S)-22,23-Dihydroxy-6β-methoxy-24-methyl-3α,5-cyclo-5α-cholestane was used as a starting material for the preparation of campestane derivatives having a 22 R,23 R-diol functionality and either a hydroxy or keto group at C-3 and labeled at C-26. The mass spectrometric behavior of the newly synthesized compounds has been studied.


1994 ◽  
Vol 40 (9) ◽  
pp. 1703-1706 ◽  
Author(s):  
W C Thompson ◽  
A Dasgupta

Abstract We prepared trifluoroacetyl, pentafluoropropyl, and heptafluorobutyl derivatives of amphetamine, methamphetamine, and 3,4-methylenedioxymethamphetamine (MDMA) in 45 s, 1 min, and 6 min, respectively, by using microwave irradiation. Conventional techniques require heating the reaction mixture for 15 min at 40 degrees C for trifluoroacetyl derivatives, 15 min at 75 degrees C for pentafluoropropyl derivatives, and 40 min at 60 degrees C for heptafluorobutyl derivatives. The mass-spectral fragmentation patterns and the gas-chromatographic retention times of the derivatives obtained by both microwave irradiation and conventional heating were similar. Perfluorooctanoyl derivatives of amphetamine can be prepared quantitatively by either heating the reaction mixture for 30 min at 60 degrees C or by 1 min of microwave irradiation. Conversion of methamphetamine and MDMA to the corresponding perfluorooctanoyl derivatives was not quantitative by either technique, although the yield of the derivative in the conventional technique was much higher.


1977 ◽  
Vol 55 (5) ◽  
pp. 831-840 ◽  
Author(s):  
Brian Maurice Lynch ◽  
Suresh Chandra Sharma

3-Oxo-s-triazolo[4,3-a]pyridine and various C-methyl derivatives (general structure 1) have been converted into the 2-β-D-ribofuranosyl species 2 and thence 4 via Friedel–Crafts catalyzed reaction with tetra-O-acetyl-β-D-ribofuranose, followed by deblocking. During the course of these reactions, rearrangements into the isomeric 3-β-D-ribofuranosyl-2-oxo-s-triazolo[1,5-a]-pyridines occur through ring-opening of the pyridine rings yielding species 3 and 5. The proportion of rearrangement products is dependent upon the position and number of the C-methyl substituents.Structural assignments for these compounds are based upon comparisons of spectroscopic properties (1H nmr, 13C nmr, uv) with model compounds from each isomeric series; structural assignments for these models are based on unequivocal mass-spectral fragmentation patterns. Unlike related triazolopyridine nucleosides with the ribose moiety attached to a pyridine nitrogen (Lynch and Sharma (1976)), there are no unusual aspects in the conformations of the nueleosides of types 4 and 5.


1972 ◽  
Vol 50 (16) ◽  
pp. 2707-2710 ◽  
Author(s):  
Larry Weiler

The mass spectra of several γ-substituted β-keto esters have been recorded and interpreted. The fragmentation patterns are compared to those of α-substituted β-keto esters and are found to be very useful in differentiating the α- and γ-substituted isomers. The mass spectral fragmentation schemes are dominated by cleavages α to the carbonyl groups and by McLafferty rearrangements.


1995 ◽  
Vol 9 (9) ◽  
pp. 778-780 ◽  
Author(s):  
Grace Karminski-Zamola ◽  
Lelja Fi??er-Jakić ◽  
Miroslav Bajić And ◽  
David W. Boykin

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