DMAP-promoted cascade C–S/C–N bonds formation approach to 1,3-thiazolidin-4-ones via annulation of β-ketothioamides with α-halocarboxylic acids at room temperature

An operationally simple and efficient one-pot straightforward method for the construction of 1,3-thiazolidin-4-ones has been developed by cyclocondensation of β-ketothioamides and an in situ generated acid anhydride from α-halocarboxylic acid in the presence of DCC at room temperature. The attractive features of this strategy include metal-free mild reaction conditions, short reaction time, and efficacy of forming consecutive C–S and C–N bonds and one ring in a single synthetic operation. Noteworthy, a Z-stereochemistry was observed for the exocyclic α-oxoketene moiety at 2-position of 1,3-thiazolidine ring.     

New Synthesis of Simvastatin

A noninfringing synthesis of simvastatin 1, starting from lovastatin 2, is presented. This synthesis features the protection of the free hydroxyl group of the lovastatin with 3,4-dihydro-2H-pyran (DHP) and opening of the lactone ring with n-BuNH₂ to afford amide 4 as a key intermediate.     

N-Alkylation of 2,6-Dichloropurine Hydrochloride with a Variety of Alcohols over Alumina Catalyst

2,6-Dichloropurine hydrochloride reacts with various types of alcohols using different alumina catalysts and converts into its N-9-alkyl-2-chloro-6-hydroxy-9H-purine products to an extent of 49–74%. The product selectivity depends on the stability of carbocation generated from the alcohol. More stable carbocation formulates both N-7 and N-9-alkyl-2,6-dichloropurine products, whereas the less stable carbocation results in exclusively N-9-alkyl-2-chloro-6-hydroxy-9H-purine. The catalytic activity of alumina prepared using the sol-gel method has larger Brunauer, Emmett, and Teller (BET) surface area and hence shows significantly greater catalytic activity than the commercially available alumina samples.     

Temperature dependent transport properties of CuInSe2-ZnO heterostructure solar Cell

Experimental study of dc and ac transport properties of CuInSe₂/ZnO heterostructure is presented. The current-voltage (I-V) and frequency dependent capacitance (C-f) characteristics of CuInSe₂/ZnO heterostructure were investigated in the temperature range 160-393 K. The heterostructure showed non-ideal behavior of I-V characteristics with an ideality factor of 3.0 at room temperature. Temperature dependent dc conductivity studies exhibited Arrhenius type behavior and revealed the presence of trap level. The C⁻²-V plot measured at frequency 50 kHz had shown non-linear behavior. An increase in capacitance with temperature was observed. The capacitance-frequency characteristics exhibited a transition between low frequency and the high frequency capacitance. As the temperature was lowered the transition occurred at lower frequencies. The frequency and temperature dependent device capacitance had shown a defect state having activation energy of 108 meV.     

Determination of copper and iron using [S,S']-ethylenediaminedisuccinic acid as a chelating agent in wood pulp by capillary electrophoresis.

A capillary electrophoresis (CE) method is described for the simultaneous determination of copper and iron after complexation with a readily biodegradable chelating agent, [S,S']-ethylenediaminedisuccinic acid (EDDS), in wood pulp. CE separation was performed in a fused-silica capillary (50 microm i.d.; total length, 65 cm) with an electrolyte containing 25 mM borate buffer and 0.5 mM CTAB at pH 7.0 and an applied voltage of -25 kV. The samples were introduced by applying a 50 mbar pressure for 2 s, and detection of the complexes was monitored at 245 nm. The methodology performance of the methods was evaluated in terms of the linearity, limit of detection (LOD), limit of quantitation (LOQ) and reproducibility. The applicability of the method was demonstrated for the analysis of copper and iron in wood pulp.     

Structural and optical properties of CuIn1−xAlxSe2 thin films prepared by four-source elemental evaporation

CuIn_1−xAl_xSe₂ (CIASe) thin films with x=0.25, 0.5 and 0.65 were prepared by four-source elemental evaporation. The structural and optical properties were investigated by X-ray diffraction, scanning electron microscopy, energy dispersive analysis, and optical transmission. The results showed that these films contain chalcopyrite structure with preferred orientation along (112) direction. The morphology, grain distribution and composition of CIASe films were studied and compared for different Al content. The optical studies revealed that the films were highly absorbing and the energy band gap calculated from transmission spectra for x=0.25, 0.5 and 0.65 were 1.2, 1.51 and 1.73 eV, respectively. The variation of Al content in the CIASe composition offered a very effective change in the optical band gap.     

Cyanine-based Fluorescent Probe for Cyanide Ion Detection

Cyanine-based probe-possessing indolium iodide and indole unit were synthesized in two-step with easy available raw material: a potential probe for the cyanide ion detection. The detecting ability of the probe was investigated and confirmed by a visual and instrumental approach. A noticeable color change from orange to colorless obtained only for cyanide ions and other added ions does not impart any changes visually and through UV and Fluorescence technique. To confirm the mechanism of sensing 1H-NMR recorded. From the result, the peak belonging to N-methyl displayed an upfield shift from 4.01 δ ppm to 2.74 δ ppm due to the disappearance of indolium iodide ion and the olefin protons peaks were shifted from 7.19 to 6.17 and 8.70 to 7.20 δ ppm confirms the nucleophilic addition of cyanide ion to the probe. Test kit from filter paper prepared for the real-time monitoring cyanide ion. The prepared strip is effective in detecting cyanide ion with a visual color change.

     

Regioselective synthesis of spiro isoxazole-oxindole-tetrahydrothiophene hybrids via cascade reactions under catalyst-free conditions

Catalyst-free synthesis of the isoxazole-spirooxindole-tetrahydrothiophene hybrids is reported. Formation of 1,4-thia-Michael and intramolecular aldol reactions were observed (instead of 1,6-thia-Michael followed by vinylogous Henry reactions) in a regioselective fashion to give new isoxazole-spirooxindole-tetrahydrothiophene hybrids with excellent yields.     

Development of Transition-Metal-Free Lewis Acid-Initiated Double Arylation of Aldehyde: A Facile Approach Towards the Total Synthesis of Anti-Breast-Cancer Agent

This work describes a mild and robust double hydroarylation strategy for the synthesis of symmetrical /unsymmetrical diaryl- and triarylmethanes in excellent yields using Lambert salt (0.2–1.0 mol%). Despite the anticipated challenges associated with controlling selective product formation, unsymmetrical diaryl- and triarylmethanes products are obtained unprecedentedly. A highly efficient gram scale reaction has also been reported (TON for symmetrical product=475 and for unsymmetrical product=390). The synthetic utility of the methodology is demonstrated by the preparation of several unexplored diaryl- and triarylmethane-based biologically relevant molecules, such as arundine, vibrindole A, turbomycin B, and certain anti-inflammatory agents. A total synthesis of an anti-breast-cancer agent is also demonstrated. Control experiments, Hammett analysis, HRMS and GC-MS studies reveal the reaction intermediates and reaction mechanism.