An organo-catalytic approach to the enantioselective synthesis of (R)-selegiline

An efficient enantioselective synthesis of (R)-selegiline has been achieved by two routes, via proline-catalyzed α-aminooxylation as well as α-amination of phenylpropanaldehyde as the key step.     

PdO nanoparticles supported on triazole functionalized porous triazine polymer as an efficient heterogeneous catalyst for carbonylation of aryl halides

A well‐defined triazole functionalized porous triazine based polymers act as solid heterogeneous catalyst after incorporating palladium oxide nanoparticles (PdO@TTAS) have been synthesized and thoroughly characterized by various techniques such as, FT‐IR, UV‐DRS, solid state ¹³C CP‐MAS, XPS, powder X‐ray diffraction, TGA, SEM and TEM analysis has been detailed illustrated. It is important to note that synthesized catalytic performance for carbonylation of aryl halides (X = I, Br) with EDC.HCl (N‐(3‐dimethylaminopropyl)‐N′‐ethylcarbodiimide hydrochloride), and formic acid was found to be an effective CO source in the presence of triethylamine as a base and DMF as a solvent medium at 80 °C for about 3 hr. The PdO@TTAS catalyst exhibits superior catalytic performance and along with good yield (up to 90%). Moreover, studying the heterogeneity and reusability of the environmentally friendly solid catalyst can be easily separated by simple filtration and then recycled for several times. In this reaction method, we avoided ligand, additive, promoters and CO gas, due to additional problem arise by using gaseous CO, highly toxic greenhouse gases and high pressurized reaction setup.     

Unique green chromatography method for the determination of serotonin receptor antagonist (Ondansetron hydrochloride) related substances in a liquid formulation,robustness by quality by design-based design of experiments approach

Serotonin receptor antagonist drug Ondansetron hydrochloride injectable formulation containing all related substances was identified and quantified by a single, simple, sensitive, eco-friendly, and green high-performance liquid chromatography method. The disseverment of all impurities was achieved with the Discovery Cyano (250 × 4.6) mm, 5 μm column. The gradient program was composed of pH 5.7 phosphate buffer as mobile phase A and acetonitrile as mobile phase B. The flow rate, column compartment temperature, and detection wavelengths were 0.9 mL/min, 30°C, and 216 nm, respectively. The method was validated as per current regulatory guidelines. The obtained %relative standard deviation for the precision results was between 0.55 and 2.72% for all impurities. The correlation coefficient values from the linearity experiment for impurities and analyte were more than 0.995. The accuracy results were obtained between 88.4 and 113.0% for all impurities. Both sample and standard solutions showed 24 h stability at benchtop and refrigerator conditions. All impurities and analytes met the specificity and mass balance for all forced degradation conditions. Quality-by-design-based design of experiments was utilized to establish the method's robustness. Method greenness was assessed by using the current advanced tool green analytical procedure index, National Environmental Methods Index, and analytical eco-scale.     

A study on the inclusion complexation of 3,4,5-trihydroxybenzoic acid with β-cyclodextrin at different pH

Effect of β-cyclodextrin (β-CD) on the absorption and fluorescence spectra of 3,4,5-trihydroxybenzoic acid (THB) have been studied buffer solutions of different pHs (pH ~1, pH ~7 and pH ~10). The study reveals that in all the above pHs THB forms 1:1 inclusion complex. The hydroxyl groups are present in the interior part of the β-CD cavity and carboxyl group is present in the hydrophilic part of the β-CD cavity. Dual luminescence is observed at pH ~1 and pH ~7 solutions which shows that intramolecular charge transfer present at these pH. The broad spectral maximum at pH ~10 indicates that intramolecular proton transfer is present in THB.     

Characterization of clinohumite by selected spectroscopic methods

Clinohumite, a humite group mineral, originated from Pamir Mountains, USSR, is used in the present work. Optical absorption, electron paramagnetic resonance (EPR), near infrared (NIR) and M?ssbauer techniques are used in the characterization of the mineral sample. The optical absorption spectrum indicates that Fe(II) impurity is present in two sites with distorted octahedral structure. NIR results are attributed to water fundamentals. EPR studies on powder sample confirm the presence of Mn(II) in three different sites and also an iron impurity. M?ssbauer studies confirm the presence of iron impurity in two different sites.     

Total synthesis of cryptopyranmoscatone B1 from 3,4,6-tri-O-acetyl-d-glucal

The first stereoselective total synthesis of the natural cryptopyranmoscatone B1 has been accomplished from 3,4,6-tri-O-acetyl-d-glucal. In addition to the double cross-metathesis reaction, a tandem nucleophilic addition-diastereoselective reduction of an in situ generated oxocarbenium cation have been used as key steps to assemble the glycoside moiety of the target molecule.     

Critical age-dependent branching Markov processes and their scaling limits

This paper studies: (i) the long-time behaviour of the empirical distribution of age and normalized position of an age-dependent critical branching Markov process conditioned on non-extinction; and (ii) the super-process limit of a sequence of agedependent critical branching Brownian motions.     

On a Singular Semilinear Elliptic Boundary Value Problem and the Boundary Harnack Principle

On a bounded C ²-domain we consider the singular boundary-value problem 1/2u=f(u) in D, u _D =, where d3, f:(0,)(0,) is a locally Hölder continuous function such that f(u) as u0 at the rate u ^–, for some (0,1), and is a non-negative continuous function satisfying certain growth assumptions. We show existence of solutions bounded below by a positive harmonic function, which are smooth in D and continuous in . Such solutions are shown to satisfy a boundary Harnack principle.     

Electronic and infrared spectral studies of manganese(III) selenito complexes

Summary Selenito manganese(III) complexes of the type MMn(SeO₃)₂ · × H₂O (where M = H⁺, NH ₄ ⁺ , K⁺, Rb⁺ and Cs⁺) have been prepared, Magnetic measurements show all these complexes to be of high spin d⁴ type, On the basis of their i.r. and electronic spectral studies and other properties, a polymeric octahedral structure involving bridging oxygen atoms has been suggested.