Synthesis of 6- and 7-acyl-4H-benzothiazin-3-ones

Synthesis of 6- and 7-substituted benzoxazin-3-ones was already described in the literature by acylation of the corresponding benzoxazin-3-ones or cyclization of the corresponding 4- or 5-acyl-2-aminophenols. This paper describes original synthetic pathways to afford the 6- and 7-acyl products in the benzothiazin-3-one series, respectively, via Stille coupling reaction and by acylation.     

A novel rearrangement reaction. A single-step conversion of tetrahydro-1-isoquinolinecarboxylic acids into 1-isoquinolones

The preparation of 2-acyl-6,7-dimethoxy-1,2,3,4-tetrahydro-1-isoquinolinecarboxamides is described. The mixed anhydride of 2-acyl-6,7-dimethoxy-1,2,3,4-tetrahydro-1-isoquinolinecarboxylic acid with isobutyl chloroformate was reacted with the corresponding hydrazines at — 10, — 15°. Besides those compounds, isoquinolones occur through a new side reaction. The structure of those products was established by ¹³C and ¹H nmr and mass spectroscopy. A possible mechanism of the reaction is discussed.     

Modulated differential scanning calorimetry

The Modulated Differential Calorimetry (MDSC) is applied to the determination of the reversibility in the cholesteryl chloride, which presents a cholesteric monotropic phase between the isotropic and crystalline states. The experimental modulation parameters that govern this method i.e. frequency, amplitude and heating/cooling rate, are determined. MDSC curves and complementary thermomicroscopical observations assign melting, crystallization and liquid cholesteric transition as non reversing, and clarification as reversing.     

New access to 4-phenyl-6H-pyrrolo[1,2-a]thieno[3,2-f]-[1,4]diazepines

Pyrrolo[1,2-a]thieno[3,2-f][1,4]diazepines were obtained in an original one step synthesis by treatment of imines 1 with paraformaldehyde in refluxing ethanol. The intermediate Mannich bases were also converted into the thienooxadiazocines 12 and the diazepine N-oxide 13 .     

Streaming current measurements in zirconia-coated capillaries

The electroosmotic flow created in zirconia-modified capillaries has been previously investigated. In this paper, we compared the electroosmotic data set with streaming current measurements and we related all these data through zeta-potential. Streaming current measurements give an excellent indication on the direction and the value of the electroosmotic mobility of an electrolyte/capillary system for a large set of experimental conditions: 2 < pH < 12, 0 < ACN < 80 %, 10(-4) M < [SO(2- )4 ] < 4 x 10(-2) M. A good correlation between zeta-potential from streaming current measurements and zeta-potential from electroosmotic mobility measurements was observed (r2 = 0.95). However, the values obtained from streaming current were always slightly lower than the one calculated from electroosmotic mobility (slope = 0.86, sigma = 0.06). In zirconia-coated capillaries the zeta-potential can be tuned from -50 to +100 mV depending on the composition of the electrolyte.     

Interactions of hairy latex particles with cationic copolymers

Interactions between polycations and core-corona particles are governed by ion-exchange reactions, entropically favored by the release of counterions. This complexation process allows the chains to penetrate into the shell, leading to adsorbed amounts greater than 1 mg m(-2). The destabilization occurs quickly, the domain of flocculation becomes larger when the concentration of monovalent salts is increased, and aggregates are composed of small and very compact clusters in a more or less self-similar structure at large scale. The adsorption of copolymers of low cationicity is characterized by still larger adsorbed amounts and layers thicker than the radius of gyration of the macromolecules. Depending on the charge content, the enhancement of the ionic strength can either promote the destabilization of the suspension or conversely induce the desorption of the chain. In pure water the structure of the flocs is long-range ordered and it becomes more heterogeneous in ionic media.     

Phosphinine stabilised gold nanoparticles; synthesis and immobilisation on mesoporous materials

The first synthesis of gold nanoparticles stabilised by a sub-stoichiometric amount of sp(2) phosphorus containing ligands was performed, as well as their immobilisation on mesostructured silica and titania hosts.     

Conformational and thermodynamic studies of alkaline subhalides M2X (M = Li, Na, K, Rb; X = F, Cl, Br, I)

Alkaline subhalides M₂X (M = Li, Na, K, Rb; X = F, Cl, Br, I) were investigated using DMol software combined with thermostatistical techniques to obtain thermodynamic data for studying the stability of these subhalides. Validation of these results was checked by establishing a link with the experimental MX-M phase diagrams by a simple empirical relation.     

Salt removal during Off-Gel electrophoresis of protein samples

The Off-Gel technology was recently described for protein fractionation in a solution placed on top of an immobilized pH gradient gel. In addition, this process was found to remove salts from the biological samples to analyze. This desalting effect is studied experimentally in a conductometric prototype cell. A simplified analytical model is developed to understand this process and a good agreement is found with the conductivity measurements. To illustrate the desalting of a biological sample, a 1 mg.mL(-1) solution of beta-lactoglobulin A in 0.1 M NaCl is subjected to electrophoresis in a single compartment Off-Gel cell. The analysis of the resulting sample by ESI-MS demonstrates the effective removal of salt. A finite element diffusion-migration model is also used to illustrate how the nonuniformity of the electric field in the cell, associated with the salt migration, can slow down the desalting process.