Characterization of molecular alkali metal iodates by mass spectrometry and matrix isolation IR spectroscopy

1992 ◽  
Vol 96 (24) ◽  
pp. 9738-9741 ◽  
Author(s):  
Karen R. Biggs ◽  
Robin A. Gomme ◽  
John T. Graham ◽  
J. Steven Ogden
Synthesis ◽  
2017 ◽  
Vol 49 (11) ◽  
pp. 2389-2393 ◽  
Author(s):  
Stefanie Pelzer ◽  
Beate Neumann ◽  
Hans-Georg Stammler ◽  
Nikolai Ignat’ev ◽  
Reint Eujen ◽  
...  

This paper describes the synthesis and comprehensive characterization of tetrakis(pentafluoroethyl)germane. In addition to a complete NMR spectroscopic characterization, including the rarely used 73Ge NMR spectroscopy, Ge(C2F5)4 was studied by IR spectroscopy, mass spectrometry as well as X-ray diffraction analysis. A 73Ge NMR investigation as well as an X-ray diffraction study of the related germane Ge(CF3)4 are also included.


2014 ◽  
Vol 67 (9) ◽  
pp. 1174 ◽  
Author(s):  
Arvid Kuhn ◽  
Daisuke Miura ◽  
Hideo Tomioka ◽  
Curt Wentrup

Methylenecycloheptadienyne 11 (heptafulvyne) is obtained very cleanly by flash vacuum thermolysis (FVT) of the diazobenzocyclobutene precursor 8 at 400°C followed by isolation as a neat solid at 77 K or in an Ar matrix at 7–10 K. Compound 11 is a yellow solid, stable till ~–100°C in the neat state. The diazo compound itself (2) is observable by IR spectroscopy following mild decomposition of the tosylhydrazone salt 1 at 115°C. FVT of 8 at 200°C also generates diazo compound 2 as observed by IR spectroscopy and on-line mass spectrometry. FVT of 8 at 600–800°C causes rearrangement of 11 to phenylacetylene 12 and benzocyclobutadiene 13. Mechanisms for the rearrangements are proposed. Facile rearrangement of benzocyclobutadiene to phenylacetylene is ascribed to chemical activation, which is also seen to be involved in the rearrangement of p-, m-, and o-phenylenebiscarbenes 25–27 to phenylacetylene 12.


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