High Yield Research Articles

Wave-Assisted Techniques, a Greener and Quicker Alternative to Synthesis of Cyclodextrin-Based Nanosponges: A Review.

The ever-increasing applications of cyclodextrin and cyclodextrin-based nanosponges in formulation development has gained much attention from researchers towards needed research in this arena. Nanosponges are three-dimensional nanoporous versatile carriers in the pharmaceutical research field because of their capability to encapsulate lipophilic and hydrophilic drugs both in their crystalline structure by inclusion and non-inclusion phenomenon. This review sheds light on the advancements made in this field and the associated patents with regard to their synthesis while zooming in on the utilization of two novel energies (Microwave and ultrasonic) in accomplishing this goal and its future thereof. Microwave and ultrasound-assisted manufacturing of cyclodextrin-based nanosponges (CDNS) has been found superior to conventional heat-dependent methods due to rapid/homogenous heating and fast kinetics, which ultimately provide the final product with high yield and crystallinity relatively rapidly. The review article also defines several facets of microwave and ultrasound-assisted nanosponge synthesis including the synergism of microwave and ultrasonic energy and the theories behind them. This hitherto unexplored microwave-ultrasonic coupling technology could be a future technology to synthesize CD-NS with a better outcome. In the recent past, these novel energy processes have been used successfully in material synthesis at an industrial scale due to their swift and streamlined synthesis attributes. Likewise, these wave-assisted methods have the full potential to materialize the concept of CD-NS from lab scale to industrial scale as a competent and versatile drug carrier, having all the prerequisite characteristics, for commercialization.

Synthesis, Characterization, and Optimization of Novel Furan-ring Fused Chalcones via Radical Cyclization of α,β-Unsaturated Ketones and Cyclic Ketone

Abstract: Novel Furan-ring Fused Chalcones (FFC) were synthesized using a radical cyclization reaction of α,β-unsaturated ketones with cyclic ketone as the model reaction to attain this goal. In this study, traditional and microwave-assisted methods for the efficient and cost-effective synthesis of furan-ring fused chalcones in mild reaction conditions are compared and optimized. The goal is to develop a reliable and adaptable synthetic technique that may be used to produce these useful chalcone derivatives quickly and effectively. The optimal experimental conditions for these reactions were carefully determined using two independent methodologies: conventional (Method A) and microwave (Method B). The results indicated that the proposed method B could be used effectively in the future to synthesize novel furans with short reaction times and acceptable yields (87-94 %), and products were purified by column chromatography and preparative thin layer chromatography (PTLC). All new compounds were characterized by 1H-NMR, 13C-NMR, LC-MS, and elemental analyses.

One-pot Synthesis of Condensed Azepines

Abstract: Azepine is a privileged nitrogen-containing ring that has been found to display a wide range of biological activities. Azepine is a valuable skeleton in designing novel compounds in medicinal chemistry due to its interesting chemical and biological properties. The study on the synthesis of this ring system engenders a fascinating area of research owing to its potential to form an active pharmacophore for De Novo exploration. In this study, conventional and domino results were compared to access the diverse set of azepines in high yield. The domino approach has revolutionized the way through which the previously impossible yet significant transformations could be conceptualized, allowing the construction of difficult materials in one step. The aim of the present mini-review is to highlight the importance of the one-pot domino reaction for the synthesis of condensed azepines. This review also presents research on this subject from the past two decades.

An Efficient Propylphosphonic Anhydride (T3P®)-Mediated MW-induced Solvent-free Rapid Synthesis of Enamino Esters and Ketones including 5, 5-Dimethyl-3-aminocyclohex-2-enones

Abstract: This work presents a clean and convenient synthesis of various β-enaminones including 5,5- dimethyl-3-aminocyclohex-2-enones, in satisfactory to excellent yields from the condensation reaction of primary amines with β -dicarbonyls by employing T3P® as a catalyst and performing the reaction under microwave irradiation and solvent-free conditions. These rapid reactions launched readily and stood a diversity of organic functional groups. A mixture of 1,3-dicarbonyl compound, primary amine and T3P® (50% in AcOEt) was irradiated for an appropriate time under microwave at 80°C. After completing the reaction (TLC) and cooling to r.t., ethyl acetate and saturated aqueous NaHCO3 solution were added. The aqueous phase was extracted ethyl acetate. The combined organic layer was washed with brine, dried over Na2SO4, and filtered, and the solvent was removed under reduced pressure to afford the product, which was recrystallized from diisopropyl ether. The presented results exhibit a better catalytic activity of T3P in the synthesis of enaminones. It could be concluded that T3P is the best catalyst as it took only a few minutes for the completion of the reaction with an excellent yield of product, which indicates T3P is more efficient, compared to other catalysts. A comparison of the efficiency of the present procedure with some heterogeneous solid catalysts was evaluated as well. Clearly, a higher yield was established in this procedure compared to other catalysts. Furthermore, the reaction of amines with dimedone was investigated as well, delivering excellent yields. The reaction catalyzed by T3P under microwave irradiation supplies a comprehensive method for the synthesis of enaminones. In this work, T3P is an effective, efficient and green catalyst, which forms the procedure economic, suitable, and safe with widespread application in the synthesis of enaminones. background: This work presents a clean and convenient synthesis of various β-enaminones incuding 5,5-dimethyl-3-aminocyclohex-2-enones in good to excellent yields from the reaction of different primary amines with 1,3-dicarbonyl compounds by employing T3P® as a catalyst and performing the reaction under microwave irradiation and solvent-free conditions. This one-pot rapid reaction proceeded readily and tolerated a variety of functional groups.

Ultrasound-Assisted Catalyst-free Synthesis of α,β -Unsaturated Amino Acid Esters and Unsaturated Amino Ketones

Introduction: Sonication has been introduced as a green and effective activation method for the selective monoamination of β-dicarbonyl compounds. The simple one-pot process resulted in different substituted β-amino-ɑ,β-unsaturated esters and ketones at room temperature with quantitative yields. Aqueous NH4OH was used as a safe and economical nitrogen source for pressurized NH3 gas. The process is considered green, accounting for not using any solvents and catalysts, besides some aqueous NH4OH-involved reactions using nontoxic water. A broad variety of useful synthetic intermediates, β- amino-ɑ,β-unsaturated esters and ketones have been prepared in short reaction time. Methods: Using this developed protocol, we were able to synthesize a series of structurally diverse β- amino-ɑ,β-unsaturated esters and unsaturated amino ketones. Results: The synthesis of target compounds was achieved in a truly green process with high atom economy and excellent yields in a catalyst-free one-pot system in an aqueous medium using simple, commercially available, inexpensive ammonium hydroxide as the source of the nitrogen. The high atom economy has been accompanied by the formation of a small amount of nontoxic waste, water. Conclusion: In conclusion, a simple, convenient, and high-yielding catalyst-free environmentally benign method was developed for the synthesis of unsaturated amino acid esters and unsaturated amino ketones.

Green and Convenient Synthesis of Pharmaceutically Active Mono and Bis-dihydroquinazolines via a One-pot Multicomponent Reaction Under Sulfamic Acid Catalysis

Introduction: Multicomponent reactions (MCRs) and green chemistry are essential criteria for the development of efficient chemical syntheses for valuable organic compounds. Method: The design, synthesis, and development of sustainable procedures for the production of novel biological and pharmaceutical molecules have gained high importance. Herein, an environmentally benign synthesis of mono- and bis-2,3-dihydroquinazolin-4(1H)-ones as pharmaceutically active compounds was carried out in good to high yields of 80-99% within 45-120 minutes. Result: The desired products were synthesized via three-component and pseudo five-component condensations of isatoic anhydride, a primary amine (aniline or ammonium acetate), and an aldehyde/dialdehyde using sulfamic acid (20%) as a solid acidic catalyst under the solvent-free condition at 100°C. Conclusion: The easy work-up procedure, metal-free and environmentally benign catalyst, green reaction conditions for performing MCRs, and high yields of pure products are some advantages of the presented protocol.

An Exceptional Valorization of CuO Nanoparticles in Ionic Liquids as an Efficient Medium for the Electrophilic Substitution of Indole Towards the Formation of Bis(indolyl)methanes

Aim: Ionic liquids are promising green solvents with simple but unique structure-related physical properties such as negligible vapour pressure, exceptional thermal conductivity, remarkable thermal stability and their suitability and inertness towards a broad range of catalytic applications. CuO NPs have been addressed as a cost-effective and a reagent of a choice that necessitates only mild reaction conditions to offer a high yield of the desired products with exceptional selectivity in a short duration of time. Therefore, in the present work, attempts have been made to explore the catalytic potentials of CuO NPs in an ionic liquid medium to synthesize biologically important bis(indolyl)methanes. Background: Catalytic explorations of metal oxide nanoparticles in ionic liquids offers a cooperative effect that has a significant impact on the kinetics as well as on the outcome of the reaction. Therefore, such catalytic systems in the present times have seized the scientific community's interest from the perspectives of sustainable development in synthetic organic chemistry. The combination of metal oxide nanoparticles with highly tunable ionic liquids is not only used to synthesize simple organic molecules but also explored in the synthesis of complex organic molecules of high commercial and biological relevance. Objectives: The current work offers a rapid and robust protocol for synthesizing bis(indolyl)methanes via electrophilic substitution reaction between indole and various aldehydes in the presence of a CuO nanoparticles-ionic liquid system. The discussion focuses on the high tolerance of different functionalities by the catalytic system leading to the synthesis of bis(indolyl)methanes. Methods: CuO NPs have been synthesized via the co-precipitation method using ionic liquid. The applicability of metal oxide nanoparticles-IL matrix was further investigated in synthesizing bis(indolyl)methanes. Results: The FT-IR absorption below 600 cm-1 and the XRD pattern showing all the peaks in the diffraction diagram revealed the formation of CuO NPs. FESEM images show the flake-shaped morphology of CuO NPs and are found to be separated from the agglomerated clusters Conclusion: Ionic liquid-CuO NPs matrix reveals good to exceptional catalytic properties, and their advancements as a catalytic system at room temperature open new avenues for synthetic organic chemists.

Effect of Herbal Kunapajala and Different Organic Manures on Plant Growth, Quality and Yield of Withania Somnifera L. Dunal

Abstract: Cultivation of medicinal plants, especially high value medicinal plants is creating new dimension in the field of agriculture. The need for developing countries to acquire technologies and techniques for programmed cultivation of medicinal plants is a current issue. Ashwagandha, the 3rd important prioritized medicinal plant listed by National Medicinal Plant Board (NMPB) is also known as Indian Ginseng. Herbal medicines strongly involve mass appeal being safer and inexpensive. The traditional use of ‘Ashwagandha was to increase energy, youthful vigour, endurance, strength, health, nurture the time elements of the body, increase vital fluids, muscle fat, blood, lymph, semen and cell production. The total alkaloid content in the roots of the Indian types has been reported to vary between 0.13 and 0.31%, though much higher yields (upto to 4.3%) have been recorded elsewhere. In all, 13 components have been obtained chromatographically. Herbal kunapajala can be used as nutrient supplement at any growth stage of crop plant. The effectiveness of herbal kunapajala is due to the breakdown of complex compounds in to lower molecular weight compounds during the fermentation of ingredients and this make available nutrients to the plants. So, this study is planned to evaluate the effect of herbal kunapajala and organic manure on ashwagandha.

Genotype by environment interaction and stability study in bread wheat (Triticum aestivum L.) genotypes in Guji Zone, Southern Ethiopia

Genotype by environment interaction and stability study in bread wheat (Triticum aestivum L.) genotypes in Guji Zone, Southern Ethiopia

Synthesis of Triphenyl Imidazole by Green chemistry approach

Synthesis of 2,3,5- Triphenyl imidazole is carried out by conventional method/ traditional method as well as green chemistry in the present study. Green chemistry is also known as micro-wave assisted synthesis. Green chemistry is the design of chemical products and process that eliminates the use and generation of hazardous substances. Using green solvent, like water, synthesis of biologically active moiety with high percentage yield as well as purity. The Percentage yield of 2,3,5- Triphenyl imidazole obtained by Green Chemistry Approach is 90.90% whereas Conventional/Traditional method produces only 69.60% of 2,3,5- Triphenyl imidazole constant concentration of all organic reagents. Hence, we concluded that green chemistry approach is environment friendly.

Complete valorization of lignocellulose with one-step acidified monophasic phenoxyethanol fractionation.

Effective fractionation of lignocelluosic biomass and subsequent valorization of all three major components under mild conditions were achieved. Pretreatment with acidified monophasic phenoxyethanol (EPH) efficiently removed 92.6% lignin and 80% xylan from poplar at 110 ℃ in 60 min, yielding high-value EPH-xyloside, EPH-modified lignin (EPHL), and a solid residue nearly purely composed of carbohydrates. After removing the grafted acetyl groups using 1% NaOH at 50 ℃, the highest enzymatic digestibility reached 92.3%. EPHL could be recovered in high yield and purity with an uncondensed structure, while xylose was converted to EPH-xyloside, a potential precursor in biomedical industries. Additionally, the acidified monophasic EPH solvent could effectively fractionate biomass from species other than hardwood, achieving over 70% delignification from recalcitrant pinewood under the same mild conditions, demonstrating the high potential of monophasic EPH pretreatment.

Kinetics and products of Thermotoga maritima β-glucosidase with lactose and cellobiose.

Galacto-oligosaccharides (GOS) are prebiotic compounds that are mainly used in infant formula to mimic bifidogenic effects of mother's milk. They are synthesized by β-galactosidase enzymes in a trans-glycosylation reaction with lactose. Many β-galactosidase enzymes from different sources have been studied, resulting in varying GOS product compositions and yields. The in vivo role of these enzymes is in lactose hydrolysis. Therefore, the best GOS yields were achieved at high lactose concentrations up to 60%wt, which require a relatively high temperature to dissolve. Some thermostable β-glucosidase enzymes from thermophilic bacteria are also capable of using lactose or para nitrophenyl-galactose as a substrate. Here, we describe the use of the β-glucosidase BglA from Thermotoga maritima for synthesis of oligosaccharides derived from lactose and cellobiose and their detailed structural characterization. Also, the BglA enzyme kinetics and yields were determined, showing highest productivity at higher lactose and cellobiose concentrations. The BglA trans-glycosylation/hydrolysis ratio was higher with 57%wt lactose than with a nearly saturated cellobiose (20%wt) solution. The yield of GOS was very high, reaching 72.1%wt GOS from lactose. Structural elucidation of the products showed mainly β(1 → 3) and β(1 → 6) elongating activity, but also some β(1 → 4) elongation was observed. The β-glucosidase BglA from T. maritima was shown to be a very versatile enzyme, producing high yields of oligosaccharides, particularly GOS from lactose. KEY POINTS: • β-Glucosidase of Thermotoga maritima synthesizes GOS from lactose at very high yield. • Thermotoga maritima β-glucosidase has high activity and high thermostability. • Thermotoga maritima β-glucosidase GOS contains mainly (β1-3) and (β1-6) linkages.

Exploring the healing power of Pistacia lentiscus stems: insights into extraction methods, polyphenolic composition, and health-promoting activities

ABSTRACT This work aimed to evaluate the effect of different extraction solvents on the polyphenolic content, antioxidant and antibacterial activity of Pistacia lentiscus stems. The results obtained show that the extraction yield depends strongly on the polarity of the solvent and the extraction method. The ethanolic extract had the highest yield in both extraction methods investigated, namely Soxhlet (R = 9.89%) and cold maceration (R = 9.20%). The free radical scavenging activity of the extracts showed that the ethanolic extract had the highest antioxidant activity in both extraction methods with an IC50 = 0.023 mg/mL (cold maceration) and an IC50 = 0.034 mg/ml (Soxhlet). The HPLC analysis of the extracts indicates that gallic acid and catechin are the major phenolic compounds. The FTIR results showed that the shift of the stretching is responsible for O-H and C-H bonding. The GC-MS analysis revealed the presence of stearic acid and palmitic acid methyl ester as main compounds. The bacterial analysis of the extracts showed that the aqueous extract represents the most active one against Staphylococcus aureus and Pseudomonas aeruginosa; on the other hand, no antifungal activity was appreciated. Overall, the results indicate that the investigated extracts might be considered valuable sources of bioactive compounds.

High External Quantum Efficiency and Dual-Band Emission of (C7H18N)3Sb2Cl9 for Sensitivity Temperature Sensing.

Organic-inorganic hybrid halides have gained attention for their ease of processing and remarkable optoelectronic properties. However, the relationship between the structure and optical properties requires further exploration. In this study, the butyltrimethylammonium cation (C7H18N+) was chosen, and seven compounds were synthesized: (C7H18N)3Sb2X9 (X = Cl, Br), (C7H18N)3Bi2X9 (X = Cl, Br, I), and (C7H18N)(C2H8N)MBr5 (M = Sb, Bi). Crystals with a single organic cation exhibit a zero-dimensional structure, while the introduction of dimethylamine ions increases the crystal dimensionality from zero-dimensional (C7H18N)3Sb2Br9 to one-dimensional (C7H18N)(C2H8N)SbBr5. Under 372 nm excitation, (C7H18N)3Sb2Cl9 showed broad orange-red single-band emission with a high photoluminescence quantum yield of 88.4% and an external quantum efficiency of up to 56.9%. A white light-emitting diode based on (C7H18N)3Sb2Cl9 achieved a high color rendering index of 96.3. Moreover, dual-band emission was observed in (C7H18N)3Sb2Cl9 under 308 nm excitation, which exhibits an absolute temperature sensitivity of 1.96 × 10-3 K-1 (320 K), and a flexible film was prepared by incorporating polydimethylsiloxane. This shows the promise of hybrid metal halides as photoluminescent materials and their possibilities for temperature sensing.

Organic or Non-organic Agriculture: Comparison of Organic and Conventional Farming Sustainability

Reduction of the level of greenhouse gas emissions from sector of agriculture are one of the serious issues across European Union. The dairy industry is responsible for generating a significant amount of emissions from enteric fermentation, manure and long-term storage. The amount of emissions produced depends highly on factors such as livestock feeding and manure management systems, feed intensity and quality. Farms that have high milk yield also produce more liquid manure, leading to an increase in overall emissions from manure management.Organic farming has been valued as one of the most suitable solutions to conventional agriculture for the achievement of climate goals. Organic farming can be described as a farming approach based on prevention, ecological processes, and the restriction of pesticides. Restricting pests and lower yields can have a negative impact on production costs and revenues. However, organic farming has lower operating costs and higher product costs, which can increase overall incomes.The research aims to evaluate the environmental, economic and social dimensions of conventional and organic farming, comparing were comparing on their integral environmental, economic and social sustainability. The core element for the sustainability assessment is the construction of the composite sustainability index using data for scientific literature, reports and statistics.

Structural formation yield of GeV centers from implanted Ge in diamond

In order to study the structural formation yield of germanium-vacancy (GeV) centers from implanted Ge in diamond, we have investigated its lattice location by using the β − emission channeling technique from the radioactive isotope 75Ge (t 1/2 = 83 min) produced at the ISOLDE/CERN facility. 75Ge was introduced via recoil implantation following 30 keV ion implantation of the precursor isotope 75Ga (126 s) with fluences around 2 × 1012–5 × 1013 cm−2. While for room temperature implantation fractions around 20% were observed in split-vacancy configuration and 45% substitutional Ge, following implantation or annealing up to 900 °C, the split-vacancy fraction dropped to 6%–9% and the substitutional fraction reached 85%–96%. GeV complexes thus show a lower structural formation yield than other impurities, with substitutional Ge being the dominant configuration. Moreover, annealing or high-temperature implantation seem to favor the formation of substitutional Ge over GeV. Our results strongly suggest that GeV complexes are thermally unstable and transformed to substitutional Ge by capture of mobile carbon interstitials, which is likely to contribute to the difficulties in achieving high formation yields of these optically active centers.

Transaminase-Catalyzed Synthesis of β-Branched Noncanonical Amino Acids Driven by a Lysine Amine Donor.

Transaminases are choice biocatalysts for the synthesis of chiral primary amines, including amino acids bearing contiguous stereocenters. In this study, we employ lysine as a "smart" amine donor in transaminase-catalyzed dynamic kinetic resolution reactions to access β-branched noncanonical arylalanines. Our mechanistic investigation demonstrates that, upon transamination, the lysine-derived ketone byproduct readily cyclizes to a six-membered imine, driving the equilibrium in the desired direction and thus alleviating the need to load superstoichiometric quantities of the amine donor or deploy a multienzyme cascade. Lysine also shows good overall compatibility with a panel of wild-type transaminases, a promising hint of its application as a smart donor more broadly. Indeed, by this approach, we furnished a broad scope of β-branched arylalanines, including some bearing hitherto intractable cyclopropyl and isopropyl substituents, with high yields and excellent selectivities.

Microgels with Immobilized Glycosyltransferases for Enzymatic Glycan Synthesis.

Glycans, composed of linked monosaccharides, play crucial roles in biology and find diverse applications. Enhancing their enzymatic synthesis can be achieved by immobilizing enzymes on materials such as microgels. Here, we present microgels with immobilized glycosyltransferases, synthesized through droplet microfluidics, immobilizing enzymes either via encapsulation or postattachment. SpyTag-SpyCatcher interaction was used for enzyme binding, among others. Fluorescamine and permeability assays confirmed enzyme immobilization and microgel porosity, while enzymatic activities were determined using HPLC. The potential application of microgels in cascade reactions involving multiple enzymes was demonstrated by combining β4GalT and α3GalT in an enzymatic reaction with high yields. Moreover, a cascade of β4GalT and β3GlcNAcT was successfully implemented. These results pave the way toward a modular membrane bioreactor for automated glycan synthesis containing the presented biocatalytic microgels.

Influence of Kluyveromyces lactis and Enterococcus faecalis on Obtaining Lactic Acid by Cheese Whey Fermentation

Cheese whey is a byproduct of the cheese industry that causes high levels of pollution in the environment, but its high lactose content means that it can be used as a source to obtain lactic acid. In this study, two strains, one belonging to a yeast and the other one to a bacteria (Kluyveromyces lactis and Enterococcus faecalis), were isolated from cheese whey and molecularly characterized, and the optimal growth conditions were determined. Then, using proteinized and deproteinized cheese whey, batch fermentation was carried out with the strains arranged in suspension and immobilized. The consumption of lactose and the production of lactic acid were measured through Brix degrees and acidity analysis. Afterwards, the lactic acid was purified, and its yield and physical and chemical characteristics were determined. It was proven that there were differences between each of the strains; arranged in free or encapsulated cells, the proteinized and deproteinized cheese wheys, under the same purification conditions, achieved different yields, colors, and densities of lactic acid. Immobilized Enterococcus faecalis had the highest yield (50.61 ± 34.94 g/L) using the deproteinized cheese whey compared to the immobilized Kluyveromyces lactis (35.70 ± 0.15 g/L) using the proteinized cheese whey.

Sweet tea extract encapsulated by different wall material combinations with improved physicochemical properties and bioactivity stability

Aim: To prepare sweet tea extract microcapsules (STEMs) via a spray-drying by applying different wall material formulations with maltodextrin (MD), inulin (IN), and gum arabic (GA). Methods: The microcapsules were characterised by yield, encapsulation efficiency (EE), particle size, sensory evaluation, morphology, attenuated total reflectance-Fourier transform infra-red spectroscopy and in vitro digestion studies. Results: The encapsulation improved the physicochemical properties and bioactivity stability of sweet tea extract (STE). MD5IN5 had the highest yield (56.33 ± 0.06% w/w) and the best EE (e.g. 88.84 ± 0.36% w/w of total flavonoids). MD9GA1 obtained the smallest particle size (642.13 ± 4.12 nm). MD9GA1 exhibited the highest retention of bioactive components, inhibition of α-glucosidase (96.85 ± 0.55%), α-amylase (57.58 ± 0.99%), angiotensin-converting enzyme (56.88 ± 2.20%), and the best antioxidant activity during in vitro gastrointestinal digestion. Conclusion: The encapsulation of STE can be an appropriate way for the valorisation of STE with improved properties.