Ultrasound assisted eco-friendly synthesis of 3-cinnamoyl coumarins using N,N'-(1,2-phenylene)bis(2-aminobenzamide) dichloro cobalt immobilized on mesoporous Al-SBA-15 as a new and recyclable catalyst

ABSTRACT

A novel mesoporous Al-SBA-15 modified by N,N'-(1,2-phenylene)bis(2-aminobenzamide) dichloro cobalt has been prepared and applied as a reusable catalyst in the 3-cinnamoyl coumarins synthesis via three-component reaction between benzaldehydes, salicylaldehydes and ethyl acetoacetate by the assist of ultrasonic irradiation. By using of the nanocatalyst and also ultrasound irradiation, the easiness and velocity of the abovementioned reaction were enhanced and an environment friendly condition was provided to synthesis of various 3-cinnamoyl coumarin compounds. The properties and structure of nanocatalyst have been specified by methods including powder X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FT-IR), transmission electron microscopy (TEM), nitrogen adsorption–desorption analysis and scanning electronic microscopy (SEM). Superiority of this novel and viable method is due to mild reaction condition, short reaction times, high yields of 3-cinnamoyl coumarins, environmentally benign, recoverability of the CoCl₂N,N'-(1,2-phenylene)bis(2-aminobenzamide)/Al-SBA-15 catalyst and reusability with important preservation in its catalytic activity.     

Insertion of tin(II) bromide into Pt–X (X = Cl,Br) bond of dimethylplatinum(IV) complexes: A novel polymorphic form of [PtBr2(bpy)]

The platinum(II) complex [PtMe₂(bpy)] (bpy = 2,2′-bipyridine) reacted with a large excess of dihaloalkanes X(CH₂)_nX (n = 1, X = Cl; n = 4, X = Br) to form the platinum(IV) complexes [PtMe₂X{(CH₂)_nX}(bpy)] (n = 1, X = Cl, 1a; n = 4, X = Br, 1b). The reaction of complexes 1a and 1b with SnBr₂ resulted in insertion of SnBr₂ into Pt–X (X = Cl, Br) bond to afford the trihalostannyl complexes [PtMe₂(SnBr₂X){(CH₂)_nX}(bpy)] (n = 1, X = Cl, 2a; n = 4, X = Br, 2b). The synthesis of such trihalostannylplatinum(IV) complexes is reported for the first time. The complex 2a was decomposed in CH₂Cl₂ solution and single crystals of [PtBr₂(bpy)] (3a) were obtained. The X-ray structure determination of 3a revealed a new polymorphic form of [PtBr₂(bpy)]. The molecules undergo a remarkable stacking along the b-axis to form a zigzag Pt?Pt?Pt chain containing both short (3.799 Å) and long (5.175 Å) Pt?Pt separations through the crystal. The crystal structure is compared to that of the yellow modification of [PtBr₂(bpy)].     

Viscoelastic characterization of compacted pharmaceutical excipient materials by analysis of frequency-dependent mechanical relaxation processes

A newly developed method for determining the frequency-dependent complex Young's modulus was employed to analyze the mechanical response of compacted microcrystalline cellulose, sorbitol, ethyl cellulose and starch for frequencies up to 20 kHz. A Debye-like relaxation was observed in all the studied pharmaceutical excipient materials and a comparison with corresponding dielectric spectroscopy data was made. The location in frequency of the relaxation peak was shown to correlate to the measured tensile strength of the tablets, and the relaxation was interpreted as the vibrational response of the interparticle hydrogen and van der Waals bindings in the tablets. Further, the measured relaxation strength, holding information about the energy loss involved in the relaxation processes, showed that the weakest material in terms of tensile strength, starch, is the material among the four tested ones that is able to absorb the most energy within its structure when exposed to external perturbations inducing vibrations in the studied frequency range. The results indicate that mechanical relaxation analysis performed over relatively broad frequency ranges should be useful for predicting material properties of importance for the functionality of a material in applications such as, e.g., drug delivery, drug storage and handling, and also for clarifying the origin of hitherto unexplained molecular processes.     

A PVC-based 1,8-diaminonaphthalen electrode for selective determination of vanadyl ion

A PVC membrane vanadyl (VO²⁺) ion-selective electrode was constructed using 1,8-diaminonaphthalen (DAN) as a neutral carrier. The electrode shows good Nernstian response for VO²⁺ ions over a wide concentration range (1.0×10⁻¹-1.0×10⁻⁵ M). The optimum composition of the membrane was 55 wt.% poly(vinylchloride), 35 wt.% 2-nitrophenyl octyl ether (NPOE), 5 wt.% ionophore, and 5 wt.% potassium tetrakis(p-chlorophenyl)borate (KTpClPB). It has relatively fast response time and can be used at least for 5 weeks without any considerable divergence in potentials. The proposed electrode revealed relatively good selectivity for VO²⁺ over wide variety of other metal ions. The electrode was used for the potentiometric titration of VO²⁺ ions with EDTA.     

Phase-controlled atom-photon entanglement in a three-level Λ-type closed-loop atomic system

We study the entanglement of dressed atom and its spontaneous emission in a three-level Λ-type closed-loop atomic system in a multi-photon resonance condition and beyond it.It is shown that the von Neumann entropy in such a system is phase-dependent,and it can be controlled by either the intensity or relative phase of applied fields.It is demonstrated that for the special case of the Rabi frequency of applied fields,the system is disentangled.In addition,we take into account the effect of Doppler broadening on the entanglement and it is found that a suitable choice of laser propagation direction allows us to obtain the steady state degree of entanglement(DEM) even in the presence of the Doppler effect.     

PVT properties of imidazolium-, phosphonium-, pyridinium- and pyrrolidinium-based ionic liquids using critical point constants

Song and Mason equation of state (EOS) with a simple modification has been extended to modelling PVT properties of ionic liquids (ILs). The considered ILs are [C₁mim][MeSO4], [C₁mim][CH₃OC₂H₅SO₄], [C₁mim][(CH₃)₂PO₄], [C₂mim][MeSO4], [C₂mim][BF₄], [C₂mim][SCN], [C₂eim][NTf₂], [C₄mim][C(CN)₃], [C₄mim][CF₃SO₃], [C₄mim][SCN], [C₅mim][NTf₂], [C₈mim][NTf₂], [(C₆H₁₃)₃P(C₁₄H₂₉)][Cl], [(C₆H₁₃)₃P(C₁₄H₂₉)][NTf₂], [(C₆H₁₃)₃P(C₁₄H₂₉)][Ac], [C₃mpyr][NTf₂], [C₄mpyr][NTf₂] and [Py][C₂H₅OC₂H₄SO₄]. Three temperature-dependent parameters in the proposed EOS have been scaled as functions of reduced temperature with the use of the law of corresponding states. It is shown that the knowledge of just critical temperature and critical density is sufficient to predict the PVT properties of these ILs. The overall average absolute deviation of calculated densities from literature values for 1347 data points of 18 ILs was found to be 0.58%. The predicted density of ILs from proposed EOS has been compared with those obtained by other literature work. Moreover, we indicate that the Zeno line regularity can well be predicted by proposed model for ILs.     

H3PMo12O40 catalyzed three-component one-pot synthesis of 4,6-diarylpyrimidin-2(1H)-ones under solvent-free conditions

<正>4,6-Diarylpyrimidin-2(1H)-one derivatives have been synthesized from three-component one-pot condensation of acetophe-none derivatives,aldehydes and urea in the presence of trimethylsilyl chloride and a catalytic amount of H_3PMo_(12)O_(40)under solvent-free conditions.     

Oxidative coupling of methane over （Na2WO4＋Mn or Ce）/SiO2 catalysts： In situ measurement of electrical conductivity

The effects of manganese oxide or ceria promoters on the performance of Na2WO4/SiO2 catalysts for oxidative coupling of methane (OCM) are reported. The OCM reaction was performed in a continuous-flow microreactor at 800 ℃, atmospheric pressure and under GHSV = 13200 ml gC-1at h-1. Catalysts were characterized by in situ conductivity measurement, FT-IR spectroscopy, XRD, SEM and temperature programmed reduction analysis. Manganese oxide promoted Na2WO4/SiO2 is considered as one of the active and selective ca...     

Heronapyrroles A-C: farnesylated 2-nitropyrroles from an Australian marine-derived Streptomyces sp

Chemical analysis of a marine-derived Streptomyces sp. (CMB-M0423) isolated from beach sand off Heron Island, Australia, yielded three new members of the rare pyrroloterpene biosynthetic structure class. Identified by detailed spectroscopic analysis as the first reported examples of naturally occurring 2-nitropyrroles, heronapyrroles A-C (1-3) displayed promising biological activity-with low to submicromolar IC(50) activity against Gram-positive bacteria but no cytotoxicity toward mammalian cell lines.