Synthesis of Highly Substituted γ‐Butyrolactones by a Gold‐Catalyzed Cascade Reaction of Benzyl Esters

Easily accessible benzylic esters of 3‐butynoic acids in a gold‐catalyzed cyclization/rearrangement cascade reaction provided 3‐propargyl γ‐butyrolactones with the alkene and the carbonyl group not being conjugated. Crossover experiments showed that the formation of the new C?C bond is an intermolecular process. Initially propargylic–benzylic esters were used, but alkyl‐substituted benzylic esters worked equally well. In the case of the propargylic–benzylic products, a simple treatment of the products with aluminum oxide initiated a twofold tautomerization to the allenyl‐substituted γ‐butyrolactones with conjugation of the carbonyl group, the olefin, and the allene. The synthetic sequence can be conducted stepwise or as a one‐pot cascade reaction with similar yields. Even in the presence of the gold catalyst the new allene remains intact.     

Pyridine solvated dioxouranium complex with salen ligand: Synthesis,characterization and luminescence properties

A new derivative of dioxouranium(VI) salen complex, [UO2(L)(pyridine)], where [L = N,N′-Bis(2-hydroxybenzylidene)-2,2-dimethyl-1,3-propanediamine] is synthesized and characterized by elemental analysis (C, H, N), FT-IR, ESI-MS spectrometry, UV/Vis, fluorescence, ¹H and ¹³C NMR spectroscopy and thermal gravimetric (TG) study. Furthermore, the single crystal X-ray diffraction measurements of the complex were carried out at 100 and 273 K. The crystal structure measurements revealed that the complex has distorted pentagonal bipyramidal geometry with uranium atom located at the centre and bonded to two phenoxy oxygen and two azomethine nitrogen in tetradenate fashion and one nitrogen from pyridine making it seven coordinated. In addition, the photoluminescence property of the complex was also recorded.     

An optical method and neural network for surface roughness measurement

The measurement of surface roughness using stylus equipment has several disadvantages. A non-contact optical method is needed for measuring the surface roughness of engineering metals with improved accuracy. One candidate for an optical method is the use of a laser source, where the laser light intensity reflected from the surface represents the surface roughness of the illuminated area. A relation can be developed between the reflected laser beam intensity and the surface roughness of the metal. The present study examines the measurement of the surface roughness of the stainless steel samples using a He-Ne laser beam. In the measurement a Gaussian curve parameter of a Gaussian function approximating the peak of the reflected intensity is measured with a fast response photodetector. In order to achieve this, an experimental setup is designed and built. In the experimental apparatus, fiber-optic cables are used to collect the reflected beam from the surface. The output of the fiber-optic system is fed to a back-propagation neural network to classify the resulting surface profile and predict the surface roughness value. The results obtained from the present study are then compared with the stylus measurement results. It is found that the resolution of the surface texture improves considerably in the case of optical method and the neural network developed for this purpose can classify the surface texture according to the control charts developed mathematically.     

Reaction of Cα,O-dilithiooximes with functionalized carbonyl compounds. Part 2 . Reaction with α-chloroketones and α,β-unsaturated aldehydes and ketones

The reaction of Cα,O-Dilithiooximes 2 and α-chloroketones afforded 5-(hydroxymethyl)-Δ²-soxazolines 4 . α,β-Unsaturated aldehydes and ketones reacted with 2 to give the corresponding acyclic 1,2-addition products 5 . The latter were cyclized with phosphorus pentoxide to 5-vinyl-Δ²-isoxazolines 6 .     

Semiquantitative determination of thirty cations by circular thin-layer chromatography

Summary A comprehensive scheme for the semiquantitative determination of 30 metal ions (Ag⁺, Pb²⁺, W⁶⁺, Tl⁺, Fe³⁺, Au³⁺, Mo⁶⁺, Ga³⁺, Sb⁵⁺, Ge⁴⁺, Te⁴⁺, Pt⁴⁺, Pd²⁺, Ru³⁺, Rh³⁺, Cu²⁺, Co²⁺, Ni²⁺, Zn²⁺, Cd²⁺, Cr⁶⁺, Mn²⁺, U⁶⁺, V⁵⁺, Sn⁴⁺, Bi³⁺, Hg²⁺, Ti⁴⁺, Se⁴⁺ and As³⁺) is described. It is based on circular thin-layer chromatographic technique. The error is ± 5% and 16 other metal ions, not included in the analysis scheme because of the non-availability of spray reagents, do not interfere. The determination of each cation has been made with different spray reagents separately and the mean error has been calculated. The analysis of the same cation with different spray reagents provides a useful check on the results. The method holds an excellent promise for the study of airborne particulates and for the determination of trace elements from blood, tissue and bone.

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Zusammenfassung Ein umfassender Analysengang für die halb quantitative Bestimmung von 30 Metallionen wurde beschrieben. Die Ringchromatographie auf Dünnschichten wurde hierzu verwendet. Der Fehler beträgt ±5%. 16 weitere Metallionen, die in Ermangelung geeigneter Sprühreagenzien in den Analysengang nicht aufgenommen wurden, stören nicht. Die Bestimmung jedes einzelnen Kations wurde mit verschiedenen Sprühmitteln vorgenommen; der mittlere Fehler wurde dann berechnet. So ist eine gute Überprüfung der Ergebnisse möglich. Das Verfahren dürfte sich für die Untersuchung der Luftverschmutzung sowie für die Bestimmung von Spurenelementen in Blut, Gewebe und Knochen eignen.

     

Three new cholinesterase-inhibiting cis-clerodane diterpenoids from Otostegia limbata

Three new tricyclic cis-clerodane type diterpenoids trivially named as limbatolide A (1), limbatolide B (2) and limbatolide C (3) have been isolated from the roots of Otostegia limbata along with two known compounds; oleanic acid and beta-sitosterol. The structure elucidation of the new compounds was based primarily on two-dimensional (2D) NMR techniques. Compounds 1-3 displayed inhibitory potential in a concentration-dependent manner against acetylcholinesterase (AChE; EC 3.1.1.7) and butyrylcholinesterase (BChE; EC 3.1.1.8) enzymes, respectively.     

Structure determination of bioactive galloyl derivatives by NMR spectroscopy

The investigation of the chemical constituents of Symplocos racemosa Roxb led to the isolation of two new glycosides, symcomoside A (1) and symcomoside B (2), together with one known glycoside, tortoside C (3), which is reported for the first time from this plant. The structures of the new compounds were determined by 1D and 2D homonuclear and heteronuclear NMR spectroscopy, from chemical evidence and by comparison with published data for closely related compounds. Symcomoside B (2) showed potent inhibitory activity against alpha-glucosidase in a concentration-dependent fashion with an IC50 value of 0.733 +/- 0.033 mM whereas symcomoside A (1) showed very weak inhibitory activity against alpha-glucosidase (9.90% in 0.70 mM).     

Spectrophotometric determination ofo- andp-phenylenediamines

Summary Cupric chloride-triphenylphosphine complex gives red color witho-phenylenediamine having maximum absorption at 505–520 nm and 0.5g/ml as visual limit of identification. The reaction is specific foro-phenylenediamine and obeys Beer's law (1 to 10g/ml). This reaction provides the basis of a new method for the Spectrophotometric determination ofo-phenylenediamine ing quantities.Ruthenium trichloride-triphenylphosphine complex gives blue color withp-phenylenediamine having maximum absorption at 580 nm and 2g/ml as visual limit of identification. On the basis of this color reaction a Spectrophotometric method for the determination ofp-phenylenediamine in hair dyes is described. The recovery of the dye from commercial preparations is better than 97%. Other organic compounds do not interfere.

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Zusammenfassung Kupfer(II)chlorid-triphenylphosphin reagiert mito-Phenylendiamin unter Rotfärbung mit maximaler Absorption bei 505 bis 520 nm und 0,5g/ml als Erfassungsgrenze. Die Reaktion ist für o-Phenylendiamin spezifisch und folgt dem Beerschen Gesetz zwischen 1 und 10g/ml. Sie dient als Grundlage für eine neue Methode der spektrophotometrischen Bestimmung von Mikrogrammengen o-Phenylendiamin.Rutheniumtrichlorid-triphenylphosphin reagiert mit p-Phenylendiamin unter Blaufärbung mit maximaler Absorption bei 580 nm und 2g/ml als Erfassungsgrenze. Auf dieser Grundlage läßt sich p-Phenylendiamin in Haarfärbemitteln bestimmen. In handelsüblichen Präparaten werden mehr als 97% des enthaltenen Farbstoffes gefunden. Andere Verbindungen stören nicht.