Some Observations on Measuring Sound Speeds in Polymers Using Time-of-Flight

Experimental Techniques - The time-of-flight method has been used to measure the longitudinal and shear wave speeds in six polymers (polyether ether ketone [PEEK], PEEK with 10% carbon fibers,...     

The crystal and molecular structures of bis (pentafluorophenyl)disulphide and bis(pentafluorophenyl)diselenide

The structures of (C₆F₅)₂S₂ and (C₆F₅)₂Se₂ have been determined by single crystal, X-ray diffraction techniques. The compounds are isostructural although the molecules are packed differently in the crystal in comparison with their phenyl analogues. Important bond lengths and angles are: SS, 2.059(4)Å; SeSe, 2.319(4)Å; SC, 1.770Å; SeC, 1.910(15)Å; SSC, 101.3(3)°; SeSeC, 98.8(1)°.     

A method to enhance porosity of micro-particles

The nuclear track technique (NTT) is used to enhance the porosity of silica micro-particles. The enhanced porosity is a result of the formation of surface and interior pores or tracks in the silica by the action of external and internal fission fragments. The fission tracks produced at the surface and within the interior of the micro-particles are a result of coating the particles with trace quantitities of uranium, instead of having trace quantities of uranium incorporated within the silica matrix.     

Mixed dialkyltin(IV) trifluoroacetates

Mixed dialkytin(IV) trifluoroacetates,Me EtSn(O₂CCF₃)₂,Et Pr ⁿ Sn(O₂CCF₃)₂ andPr ⁿ Bu ⁿ Sn(O₂CCF₃)₂ have been prepared by metathetical reactions of the corresponding dialkyltin(IV) chlorides with silver trifluoroacetate in CH₂Cl₂. They are monomeric in benzene and nonconducting inMeNO₂ andMeCN. Bidentate trifluoroacetate groups are indicated by their IR spectra.Mössbauer spectra confirmtrans-arrangement of theR-Sn-R moiety.¹H,¹⁹F NMR and mass spectra are also discussed.

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Gemischte Dialkylzinn(IV)-trifluoracetate

Zusammenfassung Die gemischten Dialkylzinn(IV)-trifluoroacetateMe EtSn(O₂CCF₃)₂,Et Pr ⁿ Sn(O₂CCF₃)₂ undPr ⁿ Bu ⁿ Sn(O₂CCF₃)₂ wurden über Metathese-Reaktionen der entsprechenden Dialkylzinn(IV)-chloride mit Silbertrifluoracetat in CH₂Cl₂ dargestellt. Sie sind monomer in Benzol und nichtleitend inMeNO₂ undMeCN. Die IR-Spektren zeigen zweizähnige Trifluoracetat-Gruppen an. DieMössbauer-Spektren bestätigen dietrans-Anordnung derR-Sn-R-Einheit. Die¹H-,¹⁹F-NMR und die Massenspektren werden ebenfalls diskutiert.

     

PROBING PHOTODYNAMIC DAMAGE IN NUCLEIC ACIDS WITH A DAMAGE-SPECIFIC DNA BINDING PROTEIN: A COMPARISON OF THE B and Z DNA CONFORMATIONS

—We have employed a damage-specific DNA binding protein from human cells as a probe for base damage in polymers irradiated with white light in the presence of methylene blue. Protein-recognizable damage is introduced only into guanine-containing polymers and quenching of damage introduction by H₂O and sodium azide suggest the involvement of a singlet oxygen mechanism. Using poly d(G-m⁵C), we have demonstrated that the left-handed double helical Z conformation is much less susceptible to guanine photooxidation than is the usual B conformation. We speculate that this difference in reactivity may reflect steric hindrance at the purine C-4 position and could provide some insight into the initial steps of the reaction between singlet oxygen and guanine in nucleic acid polymers.     

Determination of 6-N-trimethyllysine in urine by high-performance liquid chromatography

A method for determination of 6-N-trimethyllysine in urine is described. Trimethyllysine and the chemically analogous 6-N-triethyllysine internal standard were isolated from aqueous samples by microcolumn ion-exclusion chromatography. The specimens were derivatized by reaction with 1-fluoro-2,4-dinitrobenzene and reaction byproducts extracted by organic solvents. The trimethyllysine and internal standard derivatives were separated easily from other sample constituents by reversed-phase paired-ion high-performance liquid chromatography with spectrophotometric detection at 405 nm. Standard curves were linear over a sample concentration range of 10-150 nmol/ml; the detection limit corresponded with 0.1 nmol trimethyllysine injected into the chromatograph. The procedure was used for determination of trimethyllysine in human urine.     

Evidence for a doubly magic O

The decay energy spectrum for neutron unbound states in ²⁴O (Z=8$Z=8$, N=16$N=16$) has been observed for the first time. The resonance energy of the lowest lying state, interpreted as the ²⁺$2^{+}$ level, has been observed at a decay energy above 600 keV. The resulting excitation energy of the ²⁺$2^{+}$ level above 4.7 MeV, supplies strong evidence that ²⁴O is a doubly magic nucleus. The data is also consistent with the presence of a second excited state around 5.33 MeV which can be interpreted as the ¹⁺$1^{+}$ level.     

The Massless Higher-Loop Two-Point Function

We introduce a new method for computing massless Feynman integrals analytically in parametric form. An analysis of the method yields a criterion for a primitive Feynman graph G to evaluate to multiple zeta values. The criterion depends only on the topology of G, and can be checked algorithmically. As a corollary, we reprove the result, due to Bierenbaum and Weinzierl, that the massless 2-loop 2-point function is expressible in terms of multiple zeta values, and generalize this to the 3, 4, and 5-loop cases. We find that the coefficients in the Taylor expansion of planar graphs in this range evaluate to multiple zeta values, but the non-planar graphs with crossing number 1 may evaluate to multiple sums with 6^th roots of unity. Our method fails for the five loop graphs with crossing number 2 obtained by breaking open the bipartite graph K _3,4 at one edge. CNRS.     

New synthesis of (±)-cis-trikentrin A via tandem indole aryne cycloaddition/Negishi reaction. Applications to library development

We describe herein an efficient new route to the trikentrins and their related structures using a tandem 6,7-indolyne cycloaddition/Negishi cross-coupling reaction starting from a 4,6,7-tribromoindole (obtained in good yield via the Bartoli indole synthesis). The key step of this second generation route to the trikentrins is based on our observation that the 7-bromo substituent appears to undergo selective metal-halogen exchange and elimination to give the 6,7-indolyne, which is trapped in the presence of excess cyclopentadiene. Subsequent Negishi cross-coupling at the 4-bromoindole position with Et₂Zn gave directly the same intermediate obtained from our previous work. Application of this chemistry to the construction of trikentrin-related libraries using this general cycloaddition/cross-coupling tactic will also be described.     

Enantioselective determination of modafinil in pharmaceutical formulations by capillary electrophoresis, and computational calculation of their inclusion complexes

A fast capillary electrophoretic method is described for the separation and determination of the enantiomers of the novel wake-promoting agent, modafinil. Several parameters affecting the separation were studied, including the type and concentration of chiral selector, buffer pH, buffer concentration, voltage and temperature. Good chiral separation of the racemic mixture was achieved in less than 5 min with resolution factor Rs?=?2.51, using a bare fused-silica capillary and a background electrolyte (BGE) of 25 mM H₃PO₄?1 M tris solution; pH 8.0; containing 30 mg mL^?1 of sulfated-β-cyclodextrin (S-β-CD). The separation was carried out in normal polarity mode at 25 ^?C, 18 kV and using hydrostatic injection. Acceptable validation criteria for selectivity, linearity, precision, and accuracy were included. The developed method was successfully applied to the assay of enantiomers of modafinil in pharmaceutical formulations. The computational calculations for the enantiomeric inclusion complexes rationalized the reasons for the different migration times between the modafinil enantiomers.