Novel method for preparation of cyclodextrin polymers: physico-chemical characterization and cytotoxicity

The objective of this work was to optimize the synthesis procedure of soluble cyclodextrin polymers developed by Weltrowski et al. The use of the parameters indicated by the latter in our laboratory led to a lower result, which did not exceed 15 % (w/w). The new method resulted simultaneously in two fractions, a water soluble one and an insoluble one with a yield of 40 and 85 % (w/w), respectively. Only soluble cyclodextrin polymers were characterized along with the cytotoxicity study. The optimized soluble polymers were characterized by Fourier-Transform Infrared Spectrophotometer, Thermogravimetric Analyzer, Differential Scanning Calorimetry, Powder X-Ray Diffraction Analysis and Size Exclusion Chromatography. In vitro cytotoxicity against peritoneal macrophage cells of female CD1 mice showed that soluble poly-α-CD and poly-γ-CD were less cytotoxic than soluble poly-β-CD at small dose and the opposite was true at higher dose. In conclusion, temperature and time could be used to optimize the yield of polymer cyclodextrins, which will have a broad use in the drug delivery system.     

Cyclosulfamides as Constraint Dipeptides: The Synthesis and Structure of Chiral Substituted 1,2,5-Thiadiazolidine 1,1-Dioxides: Evaluation of the Toxicity

A general synthesis for the preparation of chiral N-N′ substituted 1,2,5-thiadiazolidine 1,1-dioxides has been developed beginning with proteogenic amino acid, sulfuryl chloride, and dibromoethane. The selected chemistry and spectral properties of these compounds are examined. Overall, routes described are applicable to the synthesis of a variety of constrained dipeptidal sulfamides representing novel peptidomimetic scaffolds.     

Synthèse Et Cyclisation De Carboxylsulfamides Dérivés D'amines Et D'α-Hydroxyesters. Éavaluation De L'Activité Bactéeriostatique

Abstract

Les carboxylsulfamides sont obtenus à partir de l'isocyanate de chlorosulfonyle, d'amines primaires et d'α-hydroxyesters. Après réduction alcaline, ces carboxylsulfamides sont cyclisés dans les conditions de la réaction de Mitsunobu pour conduire aux N-sulfamoyloxazolidinones chides avec des rendements élevés.

The synthesis of carboxylsulfamides was carried out starting from chlorosulfonyl isocyanate, primary amines and α-hydroxyesters. After reduction, the carboxylsulfamides were cyclised under Mitsunobu conditions giving N-sulfamoyloxazolidinones in good yields.     

Micropipette tips--the unsung heroes of mass spectrometry

Micropipette tip (tip) pipetting accuracy and precision are functions of tip manufacture consistency, morphological variation, and retained inner tip wall particulate matter. Irregular tip inner wall surfaces and retained particulate matter cause pipetting inaccuracy. Washed and unwashed tips from seven manufacturers were compared using weight by difference (six), microscopic Luxol Fast Blue staining (seven), and matrix-assisted laser desorption/onization time-of-flight (MALDI-TOF) mass spectrometry (six). Photomicrographs revealed tip irregularity and inner wall retained particulate matter. Computer model analysis was used to identify tip irregularity and retained matter. These tests established the utility of a pipette solvent wash to increase the performance and the accuracy of tips and, thus, improve the MALDI mass spectra obtained.     

Microwave-accelerated multicomponent synthesis and X-ray characterization of novel benzothiadiazinone dioxide derivatives,analogues of Monastrol

Research on Chemical Intermediates - We demonstrate here a rapid and comfortable synthetic sequence to benzothiadiazinone dioxide (six-membered cyclic sulfamide) derivatives, analogues of...     

Stabilization of Th ions into mixed-valence thorium fluoride

The unusual oxidation state +3 of the thorium has been stabilized into a lithium containing non-stoichiometric mixed-valence (III/IV) thorium fluorinated phase with formula Li_2+xTh₁₂F₅₀ (0<x<1.8). This phase is closely related to the Li_5.5Ce₁₂F₅₀ one, the structure of which has been determined from the combined single-crystal X-ray diffraction and high resolution synchrotron powder diffraction. In these phases, the Li⁺ ions can be divided into two groups and are located either in locked positions or in open channels of the three dimensional framework. The amount of Li⁺ ions in open channels can be variable, so that the afore mentioned single phase may be considered as an insertion compound. The Li⁺ insertion is accompanied by the simultaneous reduction of a part of the Th⁴⁺ ions, resulting in a mixed-valence III/IV thorium fluoride. The electrochemical insertion of Li⁺ ions into the open channels of the host matrix has been carried out at 60 °C, using an alkylcarbonate PC-LiClO₄ 1 M electrolyte. The Li⁺ and Th³⁺ contents, both in the starting composition and the Li⁺ inserted ones, were investigated by high resolution solid state ⁷Li NMR and EPR, respectively.     

Experimental and theoretical study on 3,5‐(oxo/thioxo) derivatives of 2,7‐dimethyl‐1,2,4‐triazepines–iodine molecular complexes

Intermolecular charge‐transfer (CT) spectra of 3‐thioxo‐5‐oxo‐, 5‐thioxo‐3‐oxo‐, and 3,5‐dithioxo‐ derivatives of 2,7‐dimethyl‐[1,2,4]‐triazepine 1:1 molecular complexes with molecular iodine were studied in the UV‐visible region. Equilibrium constants and free energy changes of the formed complexes were determined in solution. Ab initio calculations at HF/LANL2DZ* and MP2/LANL2DZ* were carried out to establish the nature of the complexation site, to determine the complex structures, and to examine the basicity of these compounds toward molecular iodine. The 3,5‐dithioxo‐2,7‐dimethyl‐[1,2,4]‐triazepine is the most basic one toward molecular iodine. In all cases, the complexation takes place at the heteroatom attached to position 3 of the triazepine. Hence, although in general, thiocarbonyls are stronger bases than carbonyls in the gas phase, 5‐thioxo‐2,7‐dimethyl‐[1,2,4]‐triazepin‐3‐one behaves as an oxygen base towards I₂. Experimental free energies in solution and gas‐phase computational values are linearly correlated. Copyright © 2009 John Wiley & Sons, Ltd.     

New synthesis of pentacyclic steroids by stereoselective epoxide ring opening

A stereoselective synthesis of pentacyclic steroids has been achieved. Starting from commercially available cholic acid 1, followed by asymmetric epoxidation and by stereoselective epoxide ring opening, employing nucleophilic species, the corresponding products were afforded in good yields. The compounds were being evaluated for their biological activity.