Imidomethylation of C-nucleophiles using O-phthalimidomethyl trichloroacetimidate and catalytic amounts of TMSOTf

The O-phthalimidomethyl trichloroacetimidate (1), as a latent aminomethylating agent, exhibits high electrophilicity towards a variety of C-nucleophiles in the presence of catalytic amounts of TMSOTf and mild reaction conditions. The nucleophiles include aromatics, alkenes and active methylene compounds 2-11 whereby a phthalimidomethyl group could be introduced to give compounds 12-22. Removal of the phthaloyl group gave the respective amines, β-amino ketones, and β-amino acids. The O-(trichloroacetamido)methyl trichloroacetimidate (35) was also found to be a good amidomethylating agent.     

The thermal conductivities enhancement of mono ethylene glycol and paraffin fluids by adding β-SiC nanoparticles

Changes in the thermal conductivities of paraffin and mono ethylene glycol (MEG) as a function of β-SiC nanoparticle concentration and size was studied. An enhancement in the effective thermal conductivity was found for both fluids (i.e., both paraffin and MEG) upon the addition of nanoparticles. Although an enhancement in thermal conductivity was found, the degree of enhancement depended on the nanoparticle concentration in a complex way. An increase in particle-to-particle interactions is thought to be the cause of the enhancement. However, the enhancement became muted at higher particle concentrations compared to lower ones. This phenomenon can be related to nanoparticles interactions. An improvement in the thermal conductivities for both fluids was also found as the nanoparticle size shrank. It is believed that the larger Brownian motion for smaller particles causes more particle-to-particle interactions, which, in turn, improves the thermal conductivity. The role that the base-fluid plays in the enhancement is complex. Lower fluid viscosities are believed to contribute to greater enhancement, but a second effect, the interaction of the fluid with the nanoparticle surface, can be even more important. Nanoparticle-liquid suspensions generate a shell of organized liquid molecules on the particle surface. These organized molecules more efficiently transmit energy, via phonons, to the bulk of the fluid. The efficient energy transmission results in enhanced thermal conductivity. The experimentally measured thermal conductivities of the suspensions were compared to a variety of models. None of the models proved to adequately predict the thermal conductivities of the nanoparticle suspensions.     

H<Subscript>3</Subscript>PW<Subscript>12</Subscript>O<Subscript>40</Subscript>-catalyzed one-pot synthesis of <Emphasis Type="Italic">bis</Emphasis>(indole) derivatives under silent and ultrasonic irradiation conditions in aqueous media

A convenient and direct approach has been developed for the preparation of bis(indole) derivatives by one-pot four-component condensing of indole, aldehydes and active methylene compounds in the presence of 12-tungstophosphoric acid in aqueous media under silent and ultrasound methods. The remarkable advantages are the simplicity of the experimental procedures, short reaction times and high yields with the green aspects by avoiding toxic catalysts and solvents.     

Nano‐WO3‐SO3H as a New Photocatalyst Insight Through Covalently Grafted Brønsted Acid: Highly Efficient Selective Oxidation of Benzyl Alcohols to Aldehydes

Modification of nano‐WO₃ with ?SO₃H groups as a covalently grafted solid acid reduced its band‐gap energy from 2.8 to 2.4 eV and made it an ideal nominee for photocatalytic reaction under visible light irradiation. This nano‐photocatalyst has been successfully used for the selective oxidation of different benzyl alcohols to corresponding aldehydes under blue LED irradiation. The reaction became approximately two times faster with excellent yields. It has shown that the nitrobenzene as an available industrial oxidant is applicable for photocatalytic oxidation of benzyl alcohol; remarkably high yield and selectivity have been observed.     

An efficient ultrasonic-assisted synthesis of ethyl-5-(aryl)-2-(2-alkokxy-2-oxoethylidene)-7-methyl-3-oxo-3, 5-dihydro-2H-thiazolo [3, 2-a] pyrimidine-6-carboxylate derivatives

Dihydropyrimidinone derivatives were prepared by tri-component reaction of ethyl aceto acetate, aldehydes and thiourea in the presence of modified montmorillonite nanostructure as a catalyst and used as key intermediates for the synthesis of ethyl-5-(aryl)-2-(2-alkokxy-2-oxoethylidene)-7-methyl-3-oxo-3,5-dihydro-2H-thiazolo[3,2-a]pyri midine-6-carboxylate derivatives with use of diethyl and dimethyl acetylene dicarboxylate by two methods: (a) in methanol as a solvent under ultrasonic irradiation at ambient temperature (b) in methanol as a solvent at ambient temperature (conventional magnetic stirring). Ultrasound-assisted synthesis provides excellent yields in short reaction times (15–25 min) at room temperature.     

Nanostructure of montmorillonite barrier layers: A new insight into the mechanism of flammability reduction in polymer nanocomposites

This study describes the mechanism of flammability reduction in flame-retarded polymer matrix organo-montmorillonite reinforced nanocomposites. Morphologies of untested polymer nanocomposites and char residues formed by combustion in the mass loss calorimeter are characterized by XRD and TEM techniques. It is postulated that a combination of well-dispersed montmorillonite platelets and flame retardants in the polymer matrix provides nano-structured char formation. Initial montmorillonite dispersion in flame-retarded nanocomposites is found to be a major controlling factor on formed char nanostructures. An initially intercalated structure is invariantly converted to complete montmorillonite collapse whereas an initially exfoliated structure transforms to nano-structured chars demonstrating retained exfoliation or a new state of intercalation via incomplete collapse of montmorillonite layers. It is proposed that nano-structured char formation is the effective mechanism of flammability reduction, i.e. reduction in rate of heat release during combustion, in flame-retarded polymer nanocomposites.     

Synthesis and antimicrobial activity of new 1,2,4-triazole, 1,3,4-oxadiazole, 1,3,4-thiadiazole,thiopyrane, thiazolidinone,and azepine derivatives

4-oxo-4-phenylbutanehydrazide 3 was reacted with aryl or alkyl isothiocyanates to give the corresponding N-substituted-2-(4-oxo-4-phenylbutanoyl) hydrazine-1-carbothioamide 4a-c . Cyclization of thiosemicarbazides 4a-c with sodium hydroxide led to the formation of 3-(4-sub-5-thioxo-1,2,4-triazol-3-yl)-propanone 5a-c . Desulfurization of thiosemicarbazides 4a-c by mercuric oxide afforded 3-(5-(sub-amino)-1,3,4-oxadiazol-2-yl)-propanone 6a-c . The reaction of 4a-c with phosphorus oxychloride gave 3-(5-(sub-amino)-1,3,4-thiadiazol-2-yl)-propanone 7a-c . Treatment of 4a-c with ethyl-bromoacetate or α-bromopropionic acid gave N′-(3-sub-thiazolidin-2-ylidene)-butanehydrazide 8a-c and (N′-(3-sub-oxothiazolidin-2-ylidene)-butanehydrazide 9a-c . Chlorination of oxothiazolidine-hydrazide 9a-c by phosphorus oxychloride afforded N-(3-sub-4-oxothiazolidine)-butane-hydrazonoyl-chloride 10a-c . The reaction of 10a-c with mercaptoacetyl-chloride yielded 2-((4-benzoyl-thiopyrane) hydrazono)-3-sub-thiazolidinone 11a-c . Also, reacted of 10a-c with hydrazine hydrate afforded N″-(3-sub-oxothiazolidine)-butane-hydrazon-hydrazide 12a-c . The 3-sub-2-((pyridazine) hydrazono) thiazolidinone 13a-c was obtained by cyclization of 12a-c via refluxing in DMF. The reaction and cyclized of 9a-c with chloroacetyl-chloride in ethanolic KOH afforded 1-((3-sub-4-oxothiazolidine) amino)-azepine-dione 14a-c . The chemical structures of the new compounds have been confirmed by diverse spectroscopy analyses such as IR, NMR, MS, and elemental analysis. The synthesized compounds were tested for their antimicrobial activity and these compounds were considered (Pyridazin-hydrazono-thiazolidinone 13a-c , oxothiazolidin-azepinedione 14a-c , N-thiazolidin-hydrazon-hydrazide 12a-c , and thiopyran-hydrazono-thiazolidinone 11a-c ) the most effective as antimicrobial activity.     

Pyridinium hydrobromide perbromide: a versatile catalyst for aziridination of olefins using Chloramine-T

[reaction: see text] Pyridinium hydrobromide perbromide (Py x HBr3) catalyzes effectively the aziridination of electron-deficient as well as electron-rich olefins using Chloramine-T (N-chloro-N-sodio-p-toluenesulfonamide) as a nitrogen source to afford the corresponding aziridines in moderate to good yields.