UV protection filters by dielectric multilayer thin films on Glass BK-7 and Infrasil 301

The increasing use of Ultraviolet (UV) light in medicine, industrial environments, for cosmetic use, and even in consumer products necessitates that greater attention be paid to the potential hazards of this type of electromagnetic radiation. To avoid any adverse effects of exposure to this type of radiation, four suitable protection filters were produced to block three UV bands (UVA, UVB, and UVC). The design structure of the required dielectric multilayer filters was done by optical thin film technology using the absorbing property of UV radiation for the substrates and dielectric materials. The computer analyses of the multilayer filter formulas were prepared using Macleod Software for the production processes. The deposition technique was achieved on optical substrates (Glass BK-7 and Infrasil 301) by dielectric material combinations including Titanium dioxide (Ti₂O₃), Hafnium dioxide (HfO₂), and Lima (mixture of oxides SiO₂/Al₂O₃); deposition being achieved using an electron beam gun. The output results of the theoretical and experimental transmittance values for spectral band from 200 nm to 800 nm were discussed in four processes. To analyze the suitability for use in ‘real world’ applications, the test pieces were subjected to the durability tests (adhesion, abrasion resistance, and humidity) according to Military Standard MIL-C-675C and MIL-C-48497A.     

Catalytic kinetic determination of ultratrace amounts of ruthenium(III) based on the oxidation of hematoxylin by hydrogen peroxide

A new catalytic method was described for the determination of ruthenium(III) based on its catalytic effect on the oxidation of hematoxylin by hydrogen peroxide in weakly acidic medium. The reaction was followed spectrophotometrically by measuring the absorbance of hematoxylin at 440 nm. Under the optimum conditions, ruthenium(III) can be determined in the range 5–120 ng/ml with a relative standard deviation of 1.1%. The mean value of reaction rate constant was 0.012±0.04 min^–1 and the activation energy was 10.45 kJ/mol. The method was tested for the determination of ruthenium(III) in some synthetic mixtures.     

A Convenient Regiospecific Synthesis of New Conjugated Tetrazole Derivatives via the Reaction of Dienones with the Tetrachlorosilane-Sodium Azide Reagent and their NMR Structural Assignment

Summary. Several new 1-aryl-, aralkyl-, and heteroaryl-5-(4-phenylbuta-1,3-dienyl)tetrazole derivatives and annulated tetrazole derivatives were efficiently and regiospecifically prepared in nearly quantitative yield via a facile one step reaction of dienones with a combination of tetrachlorosilane and sodium azide in acetonitrile under mild conditions. A complete structure assignment of three representative examples of the tetrazoles was achieved by advanced 2D NMR measurements including COSY, TOCSY, HSQC, HMBC, NOESY, and ROESY experiments.Received March 17, 2003; accepted March 18, 2003 Published online July 28, 2003     

A Convenient Regiospecific Synthesis of New Conjugated Tetrazole Derivatives via the Reaction of Dienones with the Tetrachlorosilane-Sodium Azide Reagent and their NMR Structural Assignment

Several new 1-aryl-, aralkyl-, and heteroaryl-5-(4-phenylbuta-1,3-dienyl)tetrazole derivatives and annulated tetrazole derivatives were efficiently and regiospecifically prepared in nearly quantitative yield via a facile one step reaction of dienones with a combination of tetrachlorosilane and sodium azide in acetonitrile under mild conditions. A complete structure assignment of three representative examples of the tetrazoles was achieved by advanced 2D NMR measurements including COSY, TOCSY, HSQC, HMBC, NOESY, and ROESY experiments.     

Enantioselective synthesis of (1S,2S)-1,2-di-tert-butyl and (1R,2R)-1,2-di-(1-adamantyl)ethylenediamines

An enantioselective synthesis of sterically congested 1,2-di-tert-butyl and 1,2-di-(1-adamantyl)ethylenediamines has been developed. Thus, diastereomerically pure trans-1-apocamphanecarbonyl-4,5-dimethoxy-2-imidazolidinones 6 and 7 were successfully prepared by optical resolution of (±)-trans-4,5-dimethoxy-2-imidazolidinone using apocamphanecarbonyl chloride (MAC-Cl) followed by stereospecific and stepwise substitution of the dimethoxyl groups using tert-butyl or 1-adamantyl cuprates to provide (4S,5S)-4,5-di-tert-butyl and (4R,5R)-4,5-di-(1-adamantyl)-2-imidazolidinones 12 and 15, respectively. Furthermore, N-acetyl 4,5-di-tert-butyl and 4,5-di-(1-adamantyl)-2-imidazolidinones 16a,b were enantioselectively deacetylated using a catalytic oxazaborolidine system to provide enantiopure 1-p-tolylsulfonyl-4,5-di-tert-butyl-2-imidazolidinones 12 and 19 and 1-p-tolylsulfonyl-4,5-di-(1-adamantyl)-2-imidazolidinones 18 and 20, respectively. Finally, N-p-tolylsulfonyl-2-imidazolidinones 12 and 15 were treated with 30 equiv of Ba(OH)₂·8H₂O to achieve ring cleavage and to provide (1S,2S)-1,2-di-tert-butylethylenediamine 3 and (1R,2R)-1,2-di-(1-adamantyl)ethylenediamine 4.     

Determination of certain trace impurities in uranium concentrates by activation analysis

A method is presented for the simultaneous determination of chromium, iron, cobalt and zinc in samples of uranium concentrates, oxides and metallic uranium by neutron-activation analysis. The method involves adequate decontamination of gross fission product activities by adsorption on silica gel, removal of uranium by solvent extraction, separation of most carrier-free rare-earth activities by coprecipitation with aluminium chloride, and, finally, fractional separation of the elements concerned by ion-exchange chromatography. The method can assay ppm of such elements in limited quantities of samples by scintillation gamma-ray spectrometric analysis with a reproducibility of 10-15%.     

Validated ecofriendly chromatographic method for quantitative determination of anti‐migraine quaternary mixture

A novel ecofriendly, cost and time saving high‐performance thin‐layer chromatographic method was developed and validated for simultaneous determination of metoclopramide, ergotamine, caffeine, and paracetamol in bulk and pharmaceutical formulation. The separation was carried out on silica gel plates, using ethyl acetate:ethanol:ammonia (9:1:0.1, v/v/v) as a developing system. Ultraviolet detection was carried out at 272 nm. The resulting retention times were 0.15, 0.36, 0.49, and 0.74 min for metoclopramide, ergotamine, caffeine, and paracetamol, respectively. The greenness profile assessment was achieved to the proposed method to evaluate its greenness characters to the environment with acceptable results. Validation parameters were checked according to International Conference of Harmonization guidelines to achieve the international requirements for quality control analysis of the proposed drugs.     

Synthesis,characterization, and biological investigation of new mixed-ligand complexes

A novel series of mixed-ligand complexes of 5,5′-{(1E,1E′)-1,4-phenelynebis(diazene-2,1-diyl)}bis(quinolin-8-ol) (H₂L₁) as a primary ligand and 4-aminoantipyrine(L₂) as a secondary ligand with Mn(II) ion were prepared using two general formulae: [Mn₂(H₂L₁)₂(L₂)₂X₄].4Cl (X = OH₂( 1 ), ONO₂⁻( 2 ), Cl=nil; OAc( 3 ), Cl = nil) and [Mn₂(H₂L₁)(L₂)₂(O₂SO₂)₂]( 4 ). Free ligands and their complexes were characterized. Electronic absorption spectra of the mixed-ligand complexes indicate a distorted octahedral geometry around the central metal ion, and the anions X⁻ are in the axial positions for all compounds. The ligands behave in a neutral bidentate manner, through nitrogen atoms and oxygen atoms of the carbonyl group (L₂), whereas H₂L₁ coordinated through nitrogen and OH groups as a neutral bidentate ligand. All complexes do not contain coordinated water molecules, but complex ( 1 ) contains four water molecules. The water molecules are removed in a single step. The complexes exhibited magnetic susceptibility corresponding to five unpaired electrons. The antimicrobial activity of the Mn(II) mixed-ligand complexes ( 1–4 ) against two gram-positive bacteria, three local gram-negative bacteria, and three fungi species was tested. Mn(II) mixed-ligand complex ( 2 ) exhibited significant antibacterial activity against Bacillus cereus, Staphylococcus aureus, Escherichia coli, Klebsiella pneumoniae, and Pseudomonas sp. Mixed-ligand complex ( 2 ) exhibited a high potential cytotoxicity against the growth of human lung cancer cells.     

Cyclodesulfurization of Substituted Thiosemicarbazides into 1,3,4-Oxadiazoles via Hydrazonoyl Chlorides

Abstract

The reaction of thiosemicarbazides 1a–h with hydrazonoyl chlorides 2a–g at ambient temperature, in the presence of triethylamine yielded, in each case, two products. The structure of these compounds was confirmed as 1,3,4-oxadiazoles 14a–h and hydrazonothioates 15a–g. The structure of 15b was confirmed through single crystal X-ray diffraction. A mechanism was proposed for this cyclodesulfurization reaction.     

Efficient Uncatalyzed Conversion of Primary and Secondary Thioamides into 1-Substituted, 5-Substituted, 1, 5-Disubstituted and Annulated Tetrazoles

Abstract

Unprecedented high-yield simple and mild conversion of primary aliphatic and aromatic thioamides into 5-substituted tetrazoles on treatment with a combination of tetrachlorosilane and sodium azide in refluxing acetonitrile has been achieved. Secondary acyclic, cyclic, and heterocyclic thioamides could also be transformed in high yields into 1-substituted, 1,5-disubstituted, or annulated tetrazoles under the same reaction condition.

GRAPHICAL ABSTRACT