An Efficient and Chemoselective Deoxygenation of Hetero Cyclic N-Oxides Using Licl/nabh4

A practical & novel reagent system L1C1/NaBH₄ is used for the deoxygenation of N-Oxides to amines is described.     

Expeditious Synthesis of Thiadiazolo Benzodiazepines Under Conventional Method and Microwave Irradiation

This article explores the use of sulfamic acid as an efficient catalyst for the one-pot synthesis of thiadiazolo 1, 5 benzodiazepines by using benzo[c][1,2,5]thiadiazole-4,5-diamine and various types of ketones in the presence of chloroform as a solvent under conventional methods and microwave irradiation. Our method is more advantageous than current methods. The catalyst (sulfamic acid) is cost effective, readily available and gives excellent yields with high purity. In comparison, the microwave irradiation method is equally as effective with a shorter reaction time and still maintaining high yields.     

Identification of liquid crystalline phases in 7O.O9 compound based on structural similarity index measure

Textural analysis is done in the case of the thermotropic liquid crystal (LC), 4-heptyloxybenzylidene-4′-nonyloxyaniline, 7O.O9, using a polarising microscope attached with a hot stage with a high-resolution camera. Natural images are highly structured: their pixels exhibit strong dependencies and carry important information about the structure of the objects. In this article, we consider the structural similarity index measure parameter computed as a function of the temperature. The results exhibit abrupt changes with temperature showing different liquid crystalline phases. This statistical image analysis is compared with the differential scanning calorimeter data and good agreement was found. The proposed methodology is very sensitive and reliable technique to identify the LC phases.     

Synthesis of substituted butenolides by the ring closing metathesis of two electron deficient olefins: a general route to the natural products of paraconic acids class

A variety of allyl acrylates possessing electron-withdrawing groups undergo RCM using the second generation Grubbs’ catalyst in the presence of a Lewis acid resulting in diverse butenolides in high isolated yields. This methodology provides a general route to the natural products of paraconic acids class, exemplified by a total synthesis of (±)-phaseolinic acid.     

Characterization of N,N‐dimethyl amino acids by electrospray ionization–tandem mass spectrometry

Methylation is an essential metabolic process for a number of critical reactions in the body. Methyl groups are involved in the healthy function of the body life processes, by conducting methylation process involving specific enzymes. In these processes, various amino acids are methylated, and the occurrence of methylated amino acids in nature is diverse. Nowadays, mass‐spectrometric‐based identification of small molecules as biomarkers for diseases is a growing research. Although all dimethyl amino acids are metabolically important molecules, mass spectral data are available only for a few of them in the literature. In this study, we report synthesis and characterization of all dimethyl amino acids, by electrospray ionization–tandem mass spectrometry (MS/MS) experiments on protonated molecules. The MS/MS spectra of all the studied dimethyl amino acids showed preliminary loss of H₂O + CO to form corresponding immonium ions. The other product ions in the spectra are highly characteristic of the methyl groups on the nitrogen and side chain of the amino acids. The amino acids, which are isomeric and isobaric with the studied dimethyl amino acids, gave distinctive MS/MS spectra. The study also included MS/MS analysis of immonium ions of dimethyl amino acids that provide information on side chain structure, and it is further tested to determine the N‐terminal amino acid of the peptides. Copyright © 2015 John Wiley & Sons, Ltd.     

Analysis of thermal,oxidative and cold flow properties of methyl and ethyl esters prepared from soybean and mustard oils

Oilseed crop with high oil content and promising ecological adaptability are potential sources for competitive biodiesel production. This study investigates the scope of utilizing biodiesel development through the methyl and ethyl ester from soybean and mustard oil as an alternative fuel. Methyl and ethyl esters of oils having different fatty acids compositions such as soybean (SOME and SOEE) and mustard oil (MUME and MUEE) were prepared by transesterification with methanol and ethanol in the presence of an alkali-KOH catalyst. The gas chromatographic (GC) analysis of oil samples revealed that primary fatty acid composition in soybean oil was linoleic acid (C_18:2, 51.93%), followed by oleic acid (C_18:1, 22.82%), palmitic acid (C_16:0, 11.56%), linolenic acid (C_18:3, 5.95%) and stearic acid (C_18:0, 4.32%). Whereas, the main components in mustard oil were erucic acid (C_22:1, 32.81%), oleic acid (C_18:1, 24.98%), eicosenoic acid (C_20:1, 10.44%), linolenic acid (C_18:3, 8.61%) and palmitic acid (C_16:0, 2.80%). The physicochemical properties (acid value, iodine value, calorific value, flash point, pour point etc.) of methyl and ethyl ester samples were estimated and found to be within the acceptable range of ASTM D6751 standards specifications. The prepared esters and oil samples were examined for cold flow properties by differential scanning calorimetry (DSC). Results revealed better cold flow properties for MUME (−2.55 °C) and MUEE (−3.10 °C) than SOME (3.21 °C) and SOEE (1.83 °C) due to more unsaturated fatty acid content in MU. Thermal and oxidative stability of samples was determined by thermogravimetric analysis (TG) and differential thermal analysis (DTA). The thermal and oxidative stability ranking of the samples was in the order of oil > methyl esters > ethyl esters.

     

Reductive amination of cyclohexanol/cyclohexanone to cyclohexylamine using SBA-15 supported copper catalysts

Amination of cyclohexanol was investigated in vapour phase over copper catalysts supported on mesoporous SBA-15. The different products identified during reductive amination of cyclohexanol reaction were cyclohexanone, cyclohexylamine, along with small amounts of N-Cyclohexylidinecyclohexylamine and dicyclohexylamine. Among several catalysts tested for the reductive amination, 5% Cu supported on SBA-15 exhibited better catalytic performance than other catalysts with 36% selectivity towards cylclohexylamine at 80% cyclohexanol conversion. The optimum reaction conditions employed to achieve the best catalyst performance were at 250 °C, 0.1 MPa of H₂/NH₃, TOS-10h. The active Cu sites, acidity of the catalyst, and effect of reaction parameters play a pivotal role in the reductive amination reaction. The prepared catalysts were characterized by XRD, BET, SEM, H₂-TPR and NH₃-TPD. The dispersion of Cu, particle size, and metal surface area (m²/g) calculated from pulse N₂O decomposition method. TPR findings reveal the presence of substantially dispersed copper oxide species at lower loadings which is easily reducible than the bulk copper oxide species found at higher Cu loadings. The acidity measurements by NH₃-TPD analysis suggest that the maximum acidic strength was obtained at 5 wt% copper on porous SBA-15, and decreased with Cu loadings. The catalytic properties are well in agreement with the findings of catalysts characterization.     

Response of colloidal liquids containing magnetic holes of different volume densities to magnetic field characterized by transmission measurement

This paper systematically investigates the response of colloidal liquids containing magnetic holes of different volume densities to magnetic field by conventional transmission measurements. It finds that the enhancement in the transmission of such a colloidal liquid under a magnetic field exhibits a strong dependence on the volume density of magnetic holes. A linear increase in the maximum enhancement factor is observed when the volume density of magnetic holes is below a critical level at which a maximum enhancement factor of ～150 is achieved in the near infrared region. Once the volume density of magnetic holes exceeds the critical level, a sharp drop of the maximum enhancement factor to ～2 is observed. After that, the maximum enhancement factor increases gradually till a large volume density of ～9%. By monitoring the arrangement of magnetic holes under a magnetic field, it reveals that the colloidal liquids can be classified into three different phases, i.e., the gas-like, liquid-like and solid-like phases, depending on the volume density of magnetic holes. The response behaviour of colloidal liquids to magnetic field is determined by the interaction between magnetic holes which is governed mainly by their volume density. A phase transition, which is manifested in the dramatic reduction in the maximum enhancement factor, is clearly observed between the liquid-like and solid-like phases. The optical switching operations for colloidal liquids in different phases are compared and the underlying physical mechanisms are discussed.