2,8,9-Trioxa-5-aza-1-sila-bicyclo[3.3.3]undecan-3-one,ein neuer typ von silatranen; darstellung und eigenschaften

A new type of silatranes (2,8,9-trioxa-5-aza-1-silabicyclo[3.3.3] undecan-3-ones) has been prepared by reaction of organotrimethoxysilanes with N-bis(2-hydroxyethyl)aminoacetic acid.The solvolytic stability compared with that of simple acyloxysilanes, the extremely decreased basicity of nitrogen and the NMR spectra prove the pentacoordination of silicon in these compounds. Basicity and NMR data are substituent-dependent.     

Polymorphic forms of lupane triterpenoid betulonic aldehyde (betulonal)

The lupane triterpenoid betulonic aldehyde [also known as betulonal; systematic name: lup‐20(29)‐en‐28‐al‐3‐one, C₃₀H₄₆O₂] is a product of betulin oxidation. Crystals were obtained from hexane [form (I)] and dimethyl sulfoxide [form (II)] solutions. Forms (I) and (II) are both orthorhombic. The molecular geometric parameters in the two forms are similar, but the structures are different with respect to the crystal packing. Polymorph (I) contains two independent molecules in the asymmetric unit, while polymorph (II) contains only one molecule, which has a disordered aldehyde group [the disorder ratio is 0.769 (4):0.231 (4)]. In each molecule, the six‐membered rings have chair conformations, whereas the cyclopentane ring in each molecule adopts an envelope conformation. All the rings in the lupane nucleus are trans‐fused. The extended structures of both polymorphs are stabilized by weak intermolecular C—H...O and van der Waals interactions. Weak intramolecular C—H...O interactions are also observed.     

Does Maternal Treatment with Zidovudine Affect Changes in Mandibles of Newborns? Laser Induced Fluorescence Study

The influence of antiretroviral drug zidovudine treatment during pregnancy on mandible development in newborn rats was studied. The fluorescence of mandibles from 7-, 14- and 28-days old individuals was measured by means of fiber-optical fluorescence analyzer with 407 nm laser excitation. Obtained results revealed disturbing effect of maternal zidovudine administration on mandible fluorescence intensity which should decrease with bone development. Small changes in fluorescence of porphyrin forms are maintaining in the first month of newborns life while the changes observed in 440–585 nm range disappear.     

Synthesis of Anellated Pyranose Derivatives on the Basis of Levoglucosenone

ABSTRACT

1,6-Anhydro-2-(dicyanomethylene)-2,3-dideoxy-4-S-ethyl-4-thio-β-D-erythro-hexopyranose (1) reacted with tosyl azide or sulfur and triethylamine to furnish the 5-aza-10, 11-dioxatricyclo[6.2.1.0^2,6]undeca-2(6),3-diene-3-carbonitrile 2 and the 10,11-dioxa-5-thiatricyclo[6.2.1.0^2,6]undeca-2(6),3-diene-3-carbonitrile 3, respectively. The reactions of 1 with arylisothiocyanates furnished the 11,12-dioxa-5-thiatricyclo[7.2.1.0^2,7]dodeca-2(7),3-diene-3-carbonitriles 4 and 5. 3 underwent cyclization with triethyl orthoformate and ammonia or hydrazine hydrate to afford the 5,7-diaza-14,15-dioxa-9-thiatetracyclo[10.2.1.0^2,10.0^3.8]pentadecatetra(tri)enes 7 and 8, respectively.     

Paramagnetic silver species in irradiated Ag−NaA zeolites. An EPR and ESEEM study

Several polymeric silver clusters have been observed in Ag_x?NaA zeolite (x=1,6) of varying water content, which was exposed to x-rays at 77 K and annealed at higher temperatures.¹⁰⁹Ag₁?NaA zeolite dehydrated at 130°C yields the dimer¹⁰⁹Ag₂ ⁺ and the trimer¹⁰⁹Ag₃ ²⁺ after irradiation at 77 K and annealing at 240 K. Owing to the use of one Ag isotope the EPR spectra of these species are highly resolved exhibitingg and hyperfine anisotropy. By irradiation of¹⁰⁹Ag_x?NaA zeolite (x=1,6) in hydrated form two new trimeric silver clusters I and II are produced. The ratio between I and II depends on the initial Ag content. ESEEM spectra of these species show interaction with aluminum nuclei of the framework and with distant water molecules. If Ag₆?NaA zeolite dehydrated at 130°C is irradiated the hexameric cluster Ag₆ ⁿ⁺ is formed. The ESEEM spectrum shows interaction only to aluminum nuclei. From ESEEM experiments on Ag₆ ⁿ⁺ with added adsorbates (D₂O, CD₃OD) it could be inferred that Ag₆ ⁿ⁺ is only stable if the neighbouring cages do not contain adsorbate molecules.     

Silver atoms and clusters in molecular sieves and clays

Electron spin resonance (ESR) and electron spin echo modulation (ESEM) studies on small paramagnetic silver clusters generated radiolytically in molecular sieves and clays are reviewed. Special attention is paid to the role of framework structure with respect to cluster nuclearity and stability. In general, geometrical size constraints play a crucial role and molecular sieves with cage-like structures with small openings between the cages such as A and rho zeolites stabilize cationic silver clusters more efficiently than channel-like zeolite structures. In addition, other factors like total cation capacity, type of cocation and/or molecular adsorbate in the cages can affect the silver agglomeration process to a great extent. The mechanism of silver agglomeration in irradiated molecular sieves and clays based on the ESR results is described as well as the reactivity of tetrameric and hexameric silver clusters with various molecular adsorbates.     

An instrumental method of solution preconcentration

Aerosol concentration before atomic-absorption measurement is achieved by use of an electrostatic trapping technique. The effects of various experimental parameters are examined, including those of voltage, trap dimensions, gas flow-rate through the trap and trapping time. It is concluded that the technique offers an inherently clean method of solution preconcentration which is capable of enhancing the signal by an order of magnitude or more.