Structural verification of a tetrahydrotetrazole compound

Tetrahydrotetrazoles are five‐membered‐ring heterocycles containing four contiguous saturated nitrogen atoms. Very few examples of such compounds have been reported in the literature. Our previous attempt at the synthesis of a member of this class of compound suggested that the N—N bonds may be more labile than expected. This finding raised the question as to whether the structures of any of the previously reported tetrahydrotetrazoles had been properly assigned. We have reproduced the synthesis of a reported tetrahydrotetrazole, namely 1,2‐di‐tert‐butyl 3‐phenyl‐1H,2H,3H,10bH‐[1,2,3,4]tetrazolo[5,1‐a]isoquinoline‐1,2‐dicarboxylate, C₂₅H₃₀N₄O₄, and have now confidently confirmed its structure via X‐ray crystallography. However, while sufficiently stable in the crystal phase, we discovered that it remains very labile in solution (having a half‐life of only 15 min at 20 °C in CDCl₃). A tentative reaction pathway for its dissociation based on ¹H NMR spectral evidence is provided.     

When random proportional subspaces are also random quotients

We discuss when a generic subspace of some fixed proportional dimension of a finite-dimensional normed space can be isomorphic to a generic quotient of some proportional dimension of another space. We show (in Theorem 4.1) that if this happens (for some natural random structures) then for any proportion arbitrarily close to 1, the first space has a lot of Euclidean subspaces and the second space has a lot of Euclidean quotients.     

Modules of piecewise polynomials and their freeness

Partially supported by NSF Grant DMS-9004123 and ARO through MSI Cornell (DAAG 29-85-C-0018)     

Conjecture de Franchetta forte

Sans résumé     

Thiol–norbornene materials: Approaches to develop high Tg thiol–ene polymers

The ability to prepare high T_g low shrinkage thiol–ene materials is attractive for applications such as coatings and dental restoratives. However, thiol and nonacrylated vinyl materials typically consist of a flexible backbone, limiting the utility of these polymers. Hence, it is of importance to synthesize and investigate thiol and vinyl materials of varying backbone chemistry and stiffness. Here, we investigate the effect of backbone chemistry and functionality of norbornene resins on polymerization kinetics and glass transition temperature (T_g) for several thiol–norbornene materials. Results indicate that T_gs as high as 94 °C are achievable in thiol–norbornene resins of appropriately controlled chemistry. Furthermore, both the backbone chemistry and the norbornene moiety are important factors in the development of high T_g materials. In particular, as much as a 70 °C increase in T_g was observed in a norbornene–thiol specimen when compared with a sample prepared using allyl ether monomer of analogous backbone chemistry. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 5686–5696, 2007     

BIOLOGICAL ACTIVITIES OF PHTHALOCYANINES-X. SYNTHESES AND ANALYSES OF SULFONATED PHTHALOCYANINES

Abstract— Synthetic methods to obtain selectively sulfonated metallo phthalocyanines are compared. Both condensation and direct sulfonation procedures lead to mixtures of mono- to tetrasulfonated products which are resolved by reverse phase liquid chromatography in buffered aqueous-methanol. The proportion of sulfonated derivatives is examined as a function of the starting reagents in the case of the condensation method, and as a function of the temperature and reaction time in the case of the direct sulfonation procedure. The number of sulfonate groups per phthalocyanine molecule is determined by oxidative degradation of the phthalocyanine ring followed by quantitative chromatographic analysis of the sulfophthalamide and phthalamide fragments.     

Analysis of aromatic compounds in gasoline with flow-switching comprehensive two-dimensional gas chromatography

A comprehensive two-dimensional gas chromatography (GC x GC) instrument has been created by coupling a flow-switching modulator and a standard gas chromatograph. The instrument was used to characterize the aromatic composition of gasoline. The high-resolution separation produced by flow-switching GC x GC allowed gasoline aromatics to be fully resolved from saturated components. The aromatic compounds were further separated into groups having the same carbon number. A standard gasoline sample was analyzed to evaluate the quantitative accuracy and precision of this technique. The data show that flow-switching GC x GC produces results that are comparable to gas chromatography-mass spectrometry (GC-MS) and thermal modulation GC x GC. The simple, low-cost, and robust nature of flow-switching GC x GC makes it an ideal technique for the routine analysis of aromatic compounds in gasoline.     

Voltammetric sizing of a sphere.

The size of a glass sphere positioned in the center of a microdisk electrode is determined by using a simple electrochemical procedure and is confirmed, additionally, by a microscopical measurement of the sphere at the time of the electrochemical measurement. The cyclic voltammetric response of the naked electrode and of the electrode with the sphere positioned in its center is recorded over a wide range of scan rates (0.002-1.5 V s(-1)). The size of the sphere is then determined by comparison of the experimental voltammogram with simulations for each individual scan rate.     

Planar Chromatographic Study of Flavonoids and Soyasaponins for Validation of Fingerprints of Desmodium adscendens of Different Origin

JPC – Journal of Planar Chromatography – Modern TLC - The flavonoid and triterpenoid soyasaponin content of the aerial parts of Desmodium adscendens from four geographical origins of...