Influence of imide functionalized organo‐modified Mg‐Al layered double hydroxide on the thermal and mechanical properties of new aliphatic‐aromatic poly (amide‐imide)

A new dicarboxylic acid modified Mg‐Al LDH (DLDH) containing imide groups was prepared and its effects on the thermal and mechanical properties of the new synthesized aliphatic‐aromatic poly (amide‐imide) (PAI) were investigated via preparation of PAI/nanocomposite films by solution casting method. The results of X‐ray diffraction (XRD), field emission‐scanning electron microscopy (FE‐SEM) and transmission electron microscopy (TEM) showed a uniform dispersion for LDH layers into the PAI matrix. For comparison, the effects of polyacrylic acid‐co‐poly‐2‐acrylamido‐ 2‐methylpropanesulfonic acid (PAMPS‐co‐PAA) modified Mg‐Al LDH (ALDH) on the PAI properties were also studied. The thermogravimetric analysis (TGA) results exhibited that the temperature at 5 mass% loss (T₅) increased from 277 °C to 310 °C for nanocomposite containing 2 mass% of DLDH, while T₅ for nanocomposite containing 2 mass% of ALDH increased to 320 °C, along with the more enhancement of char residue compared to the neat PAI. According to the tensile test results, with 5 mass% DLDH loading in the PAI matrix, the tensile strength increased from 51.6 to 70.8 MPa along with an increase in Young's modulus. Also the Young's modulus of PAI nanocomposite containing 5 mass% ALDH reduced from 1.95 to 0.81 GPa.     

Catalyst-free,aqueous and highly diastereoselective synthesis of new 5-substituted 1H-tetrazoles via a multi-component domino Knoevenagel condensation/1,3 dipolar cycloaddition reaction

An approach for the synthesis of new 5-substituted-tetrazoles via multi-component domino Knoevenagel condensation/1,3 dipolar cycloaddition reaction of carbonyl compounds, malononitrile and sodium azide in water without assistance of any catalyst has been reported. This general protocol provides a wide variety of 5-substituted 1H-tetrazoles in good yields under mild reaction conditions.     

Triphenylphosphine-Catalyzed Simple Synthesis of Dimethyl 1-Aryl-4-ethoxy-5-oxo-4,5-dihydro-1 H -pyrrole-2,3-dicarboxylates

Ethyl 2-arylamino-2-oxo-acetates undergo a complex reaction with dimethyl acetylenedicarboxylate in the presence of triphenylphosphine to produce dimethyl 1-aryl-4-ethoxy-5-oxo-4,5-dihydro-1 H -pyrrole-2,3-dicarboxylates in good yields. Dynamic NMR study of dimethyl 1-(2-methylphenyl)-4-ethoxy-5-oxo-4,5-dihydro-1 H -pyrrole-2,3-dicarboxylate shows a fairly high energy barrier ( j G p = 53.2 kJmol m 1 ) for rotation around the N-aryl single bond, which leads to an observable atropisomerism.     

Silphox [POCl3−n (SiO2) n ] as a New,Efficient, and Heterogeneous Reagent for the Synthesis of Benzimidazole Derivatives Under Microwave Irradiation

Silphox [POCl_3-n(SiO₂)_n] efficiently catalyzes the condensation of benzene-1,2-diamine with mono and dicarboxylic acids under microwave irradiation to afford benzimidazole derivatives in high yields and short reaction times.     

Spectral and Thermal Studies of Some New Metal Complexes Derived from N-[(Phenylamino)Thioxomethyl] Hydrazinocarbonyl Methyl Pyridinium Chloride (PTHMPC)

New metal complexes derived from the reaction of N-[(phenylamino)thioxomethyl] hydrazino carbonyl methyl pyridinium chloride (H₂L; PTHMPC) with some metal salts of the general formula MX₂ [(X = Cl^? and/or CH₃COO^?; M = Cd(II), UO₂(II), Mn(II) and Zr(IV)] were synthesized and characterized by elemental analyses, spectral analyses (IR, UV-vis., ¹H NMR), thermal analyses (TGA, DTG), and conductance and magnetic measurements. The results showed that the ligand exists in metal complexes either in the keto form or in the enol form. Moreover, the IR spectral data suggest that the acetate ion behaves in a monodentate manner. Semi-empirical calculations ZINDO/1, PM3, and AM1 have been used to study the molecular geometry and the harmonic vibrational spectra of the ligand and its metal complexes with the purpose of assisting the experimental assignment of the complexes. Generally, there is an agreement between the observed and the calculated spectra. Finally, the thermodynamic parameters (ΔE*, ΔH, ΔG, and ΔS) have been calculated from the data of thermal analyses (TGA and DTG).

Supplemental materials are available for this article. Go to the publisher's online edition of Phosphorus, Sulfur, and Silicon and the Related Elements to view the free supplemental file.     

Preparation and Characterization of New Optically Active Poly(amide-imide)s from N,N′-(bicyclo[2,2,2]oct-7-ene-2,3,5,6-tetra carboxylic)-bis-L-isoleucine and Aromatic Diamines

Five new optically active aromatic poly(amide-imide)s (PAIs) 5a–e were prepared from a direct polycondensation reaction of a new diacid of N,N′-(bicyclo[2,2,2]oct-7-ene-2,3,5,6-tetra carboxylic)-bis-L-isoleucine 3 with various aromatic diamines 4a–e in a medium consisting of triphenyl phosphite (TPP), calcium chloride (CaCl₂), pyridine (Py) and N-methyl-2-pyrrolidone (NMP). The polycondensation reaction produced a series of novel poly(amid-imide)s 5a–e in quantitative yields with inherent viscosities of 0.39–0.51 dL/g. The resulting polymers were fully characterized by means of ¹H-NMR, FT-IR spectroscopy, elemental analyses, inherent viscosity, solubility test, specific rotation and thermal properties of them were investigated using TGA/DTG and differential scanning calorimeter (DSC). The diacid 4 was synthesized by the condensation reaction of bicyclo[2,2,2]oct-7-ene-2,3,5,6- tetracarboxylic dianhydride 1 with L-isoleucine 2 in acetic acid solution.     

Synthesis and antitumor activity evaluation of some 1, 2, 4-triazine and fused triazine derivatives

Reactions of 3-hyrazino-5,6-diphenyl-1,2,4-triazine with various carbonyl compounds such as ethyl acetoacetate, acetylacetone, benzoin, isatin, phthalic anhydride, phenyl isocyanate and acetic anhydride were discussed. Its reactions with α, β unsaturated compounds such as arylidinemalononitrile, diethyl acetylenedicarboxylate, dibenzylidine hydrazine were studied. These reactions led to the formation of various triazine and fused-triazine derivatives. The antitumor activity of the synthesized compounds was tested against HePG2 and MCF-7 cell lines. Some of the tested compounds were most active, whereas other compounds exhibited little or no activity.