Characterization of a Novel Curcumin based Schiff base Ligand, Synthesized by Microwave Method

A new Schiff base ligand derived from curcumin and ethylenediamine has been synthesized by the microwave irradiation method. The synthesized ligand was characterized by using FT-IR, UV-VIS, Molar conductance, NMR, PL and DLS studies. The results confirmed that the successful formation of Curcumin Based Schiff Base ligand. The ligand synthesized was stable at room temperature, completely soluble in hot methanol/DMF, partially soluble in ethanol/DMSO/acetone and insoluble in water. The spectra studies of FTIR and UV-visible confirmed the formation of the azomethine group in the ligand. NMR spectrum confirmed the presence of aromatic proton, hydroxyl proton, amine proton etc in the ligand. The luminescent property of the ligand was confirmed by the photoluminescence spectroscopic method. The low molar conductance value showed the non-electrolytic nature of the ligand. The dynamic light scattering studies showed that the ligand synthesized was in nanometer scale. The structure of the ligand was also proposed based on the analysis reports.

Effect of macro and molecular initiators on the structure-property relationship of poly(ε-caprolactone)

Ring opening polymerization (ROP) of ε-caprolactone (CL) was carried out by bulk polymerization technique using stannous octoate (SO) as a catalyst and in the presence of macro or molecular initiator for 5 h under inert atmosphere with mild stirring. The % yield of poly(ε-caprolactone) (PCL) obtained was calculated and compared based on the chemical structure of macro and molecular initiators. Various analytical techniques such as FT-IR, 1H-NMR, XPS, GPC, DSC, TGA, SEM and WCA were used to characterize the PCL. The FT-IR spectrum showed the C=O stretching around ∼1725 cm−1. The aromatic proton signal of isoeugenol (IE) initiator appeared at 7–8 ppm in the proton NMR spectrum. The experimental results obtained were compared with the literature values.

HETEROCYCLIZATION OF 3-PROPARGYLSULFANYL-5 PHENYL-1,2,4-TRIAZINE: TANDEM REACTIONS WITH BROMINE LEADING TO NEW DERIVATIVES OF 7 PHENYL[1,3]THIAZOLO[3,2-B][1,2,4]TRIAZINIUM

Derivatives of 1,2,4-triazine-3-thione exhibit biological activity in a wide range. They have optoelectronic properties and can be used as synthons in synthesis of various pyridines by the Diels-Alder reaction. 1,2,4-Triazines are of the greatest interest, for organic synthesis in particular. In the present study we have established that the interaction of 3-propargylsulfanyl-5-phenyl-1,2,4-triazine, obtained by alkylation of 5-phenyl-2,3-dihydro-1,2,4-triazine-3-thione with 3-bromopropyne in acetone in the presence of triethylamine, with halogens leads to annelation of thiazole cycle. At that, [1,3]thiazolo[3,2-b][1,2,4]triazinium systems contain either endo- or exocyclic double bond in their structure, depending on the halogen type. By way of example, iodine acting on propargyl sulfide forms a dark precipitate of (3Z)-3-iodomethylene-7-phenyl-2,3-dihydro-[1,3]thiazolo[3,2-b][1,2,4]triazinium triiodide, the structure of which has been confirmed by 1H and 13C NMR spectroscopy, including two-dimensional 2D 1H-13C HSQC, HMBC and 1H-1H NOESY experiments. Treatment of the obtained triiodide by sodium iodide in acetone leads to synthesis of the corresponding monoiodide, which precipitates from the reaction mixture as a dark red precipitate. Reaction with bromine, as distinct from heterocyclization under iodine action, comprises an unusual cascade reaction including the stages of electrophile heterocyclization, bromine addition, and hydrogen bromide elimination, which leads to formation of 3-dibromomethyl-7-phenyl[1,3]thiazolo[3,2-b][1,2,4]triazinium bromide. It should be pointed out that the identifying feature of 3-propargylsulfanyl-5-phenyl-1,2,4-triazine heterocyclization under iodine and bromine action is the signal bias of the aromatic proton in a triazine ring towards weak field in the 1H NMR spectrum of the reaction products. This is presumably associated with formation of the positively charged nitrogen atom.

Structural, Thermal, Morphological, Adsorption and Catalytic Properties of Poly(BPDAH-co-ODA/PPDA)-Ag/V2O5 Nanocomposites

Thermally stable polyimides (PIs) were prepared by condensation technique at 160 ºC for 5 hours in N-methylpyrrolidone (NMP) medium under N2 atmosphere both in the presence and absence of metal (Ag) and metaloxide (MO) (V2O5) nanoparticles (NPs). The synthesized polymers are characterized by Fourier Transform Infra Red (FT-IR) spectroscopy, 1H Nuclear Magnetic Resonance (1H NMR) spectroscopy, Differential Scanning Calorimetry (DSC), Thermal Gravimetric Analysis (TGA), Scanning Electron Microscopy (SEM), Transmission Electron Microscopy (TEM), Field Emission Scanning Electron Microscopy with Energy Dispersive X-Ray (FE-SEM and EDX). The FT-IR spectrum showed a peak at 1786 cm-1 corresponding to the C=O stretching of dianhydride. The aromatic proton signals appeared between 6.7 and 7.5 ppm in the 1H-NMR spectrum of the resultant PIs. The oxydianiline (ODA) based PI with Ag NP loaded system exhibited the highest Tg value. The apparent rate constant values for the adsorption and catalytic reduction of p-nitrophenol (PNP), Cr6+ and rhodamine 6G (R6G) dye were determined with the help of UV-visible spectrophotometer. Among the catalysts, the system loaded with V2O5 NP has higher kapp values. The experimental results are critically analyzed and compared with the previously available literature values. Copyright © 2020 BCREC Group. All rights reserved

Synthesis of highly stable metal-containing extra-large-pore molecular sieves

The isomorphic substitution of two different metals (Mg and Co) within the framework of the ITQ-51 zeotype (IFO structure) using bulky aromatic proton sponges as organic structure-directing agents (OSDAs) has allowed the synthesis of different stable metal-containing extra-large-pore zeotypes with high pore accessibility and acidity. These metal-containing extra-large-pore zeolites, named MgITQ-51 and CoITQ-51, have been characterized by different techniques, such as powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectrometry, UV–Vis spectroscopy, temperature programmed desorption of ammonia and Fourier transform infrared spectroscopy, to study their physico-chemical properties. The characterization confirms the preferential insertion of Mg and Co atoms within the crystalline structure of the ITQ-51 zeotype, providing high Brønsted acidity, and allowing their use as efficient heterogeneous acid catalysts in industrially relevant reactions involving bulky organic molecules.

Supra-molecular assembly of aromatic proton sponges to direct the crystallization of extra-large-pore zeotypes

The combination of different experimental techniques, such as solid 13 C and 1 H magic-angle spinning NMR spectroscopy, fluorescence spectroscopy and powder X-ray diffraction, together with theoretical calculations allows the determination of the unique structure directing the role of the bulky aromatic proton sponge 1,8- bis (dimethylamino)naphthalene (DMAN) towards the extra-large-pore ITQ-51 zeolite through supra-molecular assemblies of those organic molecules.