Regioselective cyclization of chloroacylaminobenzenesulfonamide derivatives

Chloroacylaminobenzensulfonamides regioselectively thermally cyclize under solvent free conditions to 1,2,4-benzothiadiazines with five- and six-membered rings fused on face b.     

High-performance liquid chromatographic determination of diltiazem in human plasma after solid-phase and liquid–liquid extraction

A selective, sensitive, and accurate high-performance liquid chromatographic method for determination of diltiazem in plasma samples has been developed and validated. The effects of mobile phase composition, buffer concentration, mobile phase pH, and concentration of organic modifiers on retention of diltiazem and internal standard were investigated. Solid-phase and liquid–liquid extraction were examined and proposed for isolation of the drug and elimination of endogenous plasma interferences. A 5 m Lichrocart Lichrospher 60 RP-select B chromatographic column was used; the mobile phase was acetonitrile–0.025 mol L^–1 KH₂PO₄ (pH 5.5), 35:65 ( v / v) at a flow-rate of 1.5 mL min^–1. The detection wavelength was 215 nm. The calibration plots were linear in the concentration range 20.0–500.0 ng mL^–1. The method has been implemented to monitor diltiazem levels in patient samples.     

Bis­(tetra­methyl­ammonium) hexa­molyb­date hydrate, [(CH3)4N]2[Mo6O19]·H2O

The crystal and molecular structure of the title compound, (C₄H₁₂N)₂[Mo₆O₁₉]·H₂O, has been determined from X‐ray diffraction data. The poly­oxo­anion [Mo₆O₁₉]^2? is built up from six distorted MoO₆ octa­hedra sharing common edges and one common vertex at the central O atom, and has crystallographic m3m (O_h) symmetry. The cation has crystallographic 3m symmetry.     

Effects of annealing on crystallinity and phase behaviour of PET/PC block copolymers

The effects of the annealing on the properties of PET/PC block copolymers, obtained by reactive blending in the presence of different catalysts and for different mixing times, have been studied. The annealing, performed in conditions that promote the crystallization, has been used to better understand the role of block length in determining the phase behaviour. The copolymers characterized by blocks with molecular weight larger than 8000 are able to reorganize towards more ordered domains. This rearrangement maintains the phase separation, as two crystalline phases are present before and after annealing, due to the immiscibility of long blocks. In copolymers characterized by blocks with molecular weight equal to about 2500, that is the higher limit for the miscibility in the amorphous state in PET/PC block copolymers studied in this work, the rearrangement of the chains during annealing causes a phase separation leading to two crystalline phases. Only in the copolymers with molecular weight of blocks lower than 1500, the very short block length hinders the crystallization: therefore, only in this case a phase separation does not take place after annealing.     

RE3Ga9Ge (RE=Y, Ce, Sm, Gd and Yb): compounds with an open three-dimensional polygallide framework synthesized from liquid gallium

The RE₃Ga₉Ge compounds (RE=Y, Ce, Sm, Gd and Yb) were synthesized at 850°C in quantitative yield from reactions containing excess liquid Ga. The orthorhombic crystal structure is characterized by a unique three-dimensional open Ga framework with parallel straight tunnels. In the tunnels, inserted are arrays of the RE atoms together with interpenetrated monoatomic RE-Ga-Ge planes. A complex disordered arrangement of the RE and Ga atoms is observed in the monoatomic plane. Depending on the extent of disorder, the crystal structure could be presented either in a sub-cell (no ordering) or in a super-cell (partial ordering). Single-crystal X-ray data for Ce₃Ga₉Ge sub-structure: space group Immm, Z=2, cell parameters a=4.3400(12) Å; b=10.836(3) Å; and c=11.545(3) Å; super-structure: space group Cmma, Z=8, cell parameters a=8.680(3) Å; b=23.090(7) Å; and c=10.836(3) Å. The refinement based on the full-matrix least squares on F_o²[I>2σ(I)] converged to final residuals R₁/wR₂=0.0226/0.0528 and 0.0729/0.1569 for the sub- and super-structures, respectively. The relationship between the disordered sub-structure and partially ordered super-structure is discussed. Magnetic susceptibility measurements show Curie-Weiss behavior at the temperatures above 30 K with the negative Weiss constants Θ=−49(1) and−7.7 K for Gd and Ce analogs, respectively. An antiferromagnetic transition is observed in the Gd analog at T_N=26.1 K. The μ_eff obtained for both analogs is close to the RE³⁺ free-ion value.     

Benzocoumarins from the rhizomes of Juncus acutus

Investigation of the ethyl acetate extract of Juncus acutus rhizomes revealed seven benzocoumarins, probably derived from oxidation of phenanthrenes already isolated from the plant. The structures were determined by means of spectroscopic methods. The anti-algal activity of the isolated compounds tested on the green alga Pseudokirchneriella subcapitata are reported here.