Microwave‐Assisted Synthesis of Spiro‐Isoxazolidines

Solvent‐free synthesis of spiro‐isoxazolidines (exclusively endo‐diastereoisomers) through [3 + 2] cycloaddition of N‐cyclohexylidene N‐phenyl nitrones with cyclic dipolarophiles under microwave irradiation is described.     

Heteropoly Acids as Heterogeneous and Reusable Catalyst for α-Thiocyanation of Ketones

Simple, efficient, and mild method for α-thiocyanation of ketones in presence of heteropolyacid has been developed. This methodology offered α-oxothiocyanates in good to excellent yields at room temperature in a highly selective manner. The catalyst could be efficiently recovered from the reaction and reused.     

Micellar Enhanced Ultrafiltration of Reactive Black 5 from Aqueous Solution by Cationic Surfactants

Reactive black 5 (RB-5) dye was removed from a water stream using two cationic surfactants, cetyltrimethylammonium bromide (CTAB) and cetylpyridinium chloride (CPC), via micellar enhanced ultrafiltration. Three membranes with different pore size were used for the determination of rejection coefficient and permeate flux of the solution at 1.5 bar trans-membrane pressure (TMP). The two surfactants (CPC and CTAB) played an almost negligible role in rejection efficiency with 5000 and 10,000 molecular weight cut-off membrane (MWCO), respectively. In this case, high rejection and low permeate flux was the result of a larger molecular size of RB-5 DYE being retained by comparatively smaller sized pores of membrane via ultrafiltration. However, CPC and CTAB surfactants showed 83% and 98% rejection coefficient, respectively, at a concentration greater than their CMC values against 30,000 MWCO. Permeate flux remained low and constant in presence of 5000 and 10,000 MWCO with a small variation against 30,000 MWCO for the two surfactants, thereby no appreciable effect on both surfactant concentrations on concentration polarization was estimated. Thus, RB-5 dye alone was determined to be responsible for membrane plugging or concentration polarization and ultimately for low permeate flux. The effect of trans-membrane pressure was also investigated during this study.     

Spectrophotometric method for determination of atrazine and its application to commercial formulations and real samples

A simple sensitive spectrophotometric method has been developed for the determination of atrazine in herbicide formulations and real samples. The method was based on the reaction of atrazine with pyridine to form a quaternary halide which in the presence of alkali forms a carbinol base. The heterocyclic ring of the carbinol base breaks and forms the glutaconic dialdehyde. The glutaconic dialdehyde group was coupled with sulfanilic acid to form a yellow coloured product having λ _max 450 nm or coupled with aniline to form a orange red coloured product having λ _max 480 nm. The Beer's law was obeyed over the range from 0.1 to 25 µg mL^?1 and molar absorptivity 1.5 × 10⁴ L mol^?1 cm^?1 for sulfanilic acid, and from 0.08 to 12 µg mL^?1 and molar absorptivity 1.3 × 10⁴ L mol^?1 cm^?1 for aniline were observed. The reaction conditions and other analytical parameters were optimised. The proposed method has been successfully applied for the analysis of commercial formulations and real samples.     

Determination of Trace Elements in Tea and Coffee by Neutron Activation Analysis

Thermal neutron activation analysis, a high-resolution Ge(Li) gamma-ray spectrometer, and an IBM 360/67 digital computer were used to determine the concentration of Na, K, Sc, Cr, Mn, Fe, Co, Cu, Zn, Se, Br, Rb, Sb, Cs, and Hg in ground coffee and tea. This nondestructive multielement technique requires neither pre- nor postirradiation chemistry and eliminates problems of reagent contamination. The method is simple, precise and sensitive to 15 elements. Interferences from fast neutron (n, p) and (n, α) reactions are small and, if necessary, corrections may be applied easily. This technique can be applied to percolated tea and coffee.     

Synthesis, structure, and electronic calculations of group VII substituted pyridazines

A series of 5,6-fused ring cyclopentadienyl tricarbonyl manganese and rhenium complexes, [M(CO)₃{η ⁵-1,2-C₅H₃(1,4-(R)₂N₂C₂}] (2a–3d) were isolated by employing an off-metal ring closure route. Reacting thallium cyclopentadienide (Cp) salts (1a–d) with [MBr(CO)₅] (M = Mn, Re) provided pyridazyl complexes (2a–3d) in high yield (75–99 %). Spectroscopic characterization (NMR, IR, MS) confirmed the identity of the desired organometallic pyridazines. The off-metal synthetic pathway employed did improve upon the isolation of these complexes as compared to previously reported routes. The molecular and electronic structure of complexes 2a–3d and their optimal energy structures have been characterized with quantum chemistry calculations. Vibrational frequencies calculated were compared to their experimental counterparts. The excited state calculations predict that the dominant low-energy transition involves a ligand-to-metal charge transfer.     

Synthesis of Sugars From D-Ribonolactone. II. An Alternative Synthesis of D-Erythrose

D-Erythrose was synthesized in four steps from D-ribono-1,4-lactone via the 3,5-O-benzylidene derivative of the latter compound. Reduction of the benzylidene D-ribonolactone, and periodate cleavage of the resulting 3,5-O-benzylidene-D- ribitol were performed in a one-flask reaction. The ensuing 2,4-O-benzylidene-D-erythrose was hydrolyzed with 10% acetic acid to obtain syrupy D-erythrose.     

Vasicine as tridentate ligand for enantioselective addition of diethylzinc to aldehydes

The first report of natural l-vasicine as tridentate chiral ligand for the enantioselective addition of diethylzinc to a variety of aliphatic and aromatic aldehydes is described. The ligand generates R-isomer of the secondary alcohols upto 98% ee. The quinazoline structure possibly imparts rigidity to the ligand and hence, consistently high enantioselectivity. The importance of the quinazoline ring was also supported by the reaction with other related ligands, partially lacking the structural features, thus resulting in poor enantioselectivity.     

Steric and Electronic Influence on the Coordination Aptitude of 4‐Formylpiperazine‐1‐Carbodithioate Towards Triorganotin(IV) Moieties

A fascinating ligand, 4‐formylpiperazinium 4‐formylpiperazine‐1‐carbodithioate (L‐salt) has been reacted with two electronically and sterically different trimethyltin(IV) chloride and triphenyltin(IV) chloride. The complexes 1 and 2 were characterized by elemental analysis, spectroscopic techniques, and X‐ray single crystal analysis. The latter technique confirmed the polymeric and monomeric nature of 1 and 2 , respectively. Both 1 and 2 showed intriguing molecular packing properties in the solid state. However, the packing of 1 is more interesting and unique where one‐dimensional polymer chains self assemble in two‐over‐two saltire‐shaped fashion to provide an overall multilayered structure. The different behavior of L toward two different tin(IV) compounds can be attributed to different electronic and steric environments around metal center.     

Synergistic effect of aluminum trihydrate and zirconium hydroxide nanoparticles on mechanical properties,flammability, and thermal degradation of polyester/jute fiber composite

Cellulose - This study focuses on the synergistic effects of hydroxide based nanoparticles namely aluminum trihydrate (ATH) and zirconium hydroxide (ZHO) on the mechanical characteristics, thermal...